摘要:

AbstractThe reaction of 4‐chloro‐5‐cyano‐2‐methylthiopyrimidine (I) with ethyl mercaptosuccinate (II) in refluxing ethanol containing sodium carbonate has afforded diethyl 3‐amino‐2‐(methyl‐thio)‐7H‐thiopyrano[2,3‐d]pyrimidine‐6,7‐dicarboxylate (IV). Displacement of the methylthio group in IV with hydrazine gave the corresponding hydrazino derivative which underwent Schiff base formation with benzaldehyde or 2,6‐dichlorobenzaldehyde. Treatment of IV in refluxing acetic anhydride afforded the corresponding diacetylated amino derivative. Partial saponification of IV with sodium hydroxide gave 5‐amino‐2‐(methylthio)‐7H‐thiopyrano‐[2,3‐d]pyrimidine 6,7‐dicarboxylic acid 6 ethyl ester (VIII). The reaction of 4‐amino‐6‐chloro‐5‐cyano‐2‐phenylpyrirnidine (XI) with II resulted in the formation of ethyl 4‐amino‐6‐(ethoxy‐carbonyl)‐5,6‐dihydro‐5‐amino‐2‐phenylthieno[2,3‐d]pyrimidine‐6‐acetate (XIII) which when subjected to hydrolysis gave ethyl 4,5‐diamino‐2‐phenylthieno[2,3‐d]pyrimidine‐6‐acetate isolated as the hydrochloride (XIV). Diazotization of IV with sodium nitrite in acetic acid unexpectedly afforded diethyl 5‐(acetyloxy)‐6,7‐dihydro‐6‐hydroxy‐2‐(methylthio)‐5H‐thio

ISSN:0022-152X    

DOI:10.1002/jhet.5570140301

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

Abstractp‐Nitrobenzoylphenylacetylene (I) reacted with acylhydrazines (IIa‐d) to give the corresponding hydrazones (VIa‐d), which when treated with acetic anhydride, gave the same substituted pyrazole (VII). Hydrolysis of the latter with methanolic potassium hydroxide gave the pyrazole derivative (IX).The reaction of I with ethyl and phenyl hydrazinecarboxylates (IIe,f) led to the formation of the hydrazones (VIe) and (VIf), respectively, whereas with methyl‐ and phenylhydrazines it produced the pyrazoles (X) and (XI), respectively. However, guanidine hydrochloride gave with acetylenic ketone (I), the pyrimidi

ISSN:0022-152X    

DOI:10.1002/jhet.5570140302

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

AbstractA number of substituted 2H‐pyrazolo[3,4‐d]pyridazines, pyridazin‐7(6H)ones, and ‐pyrid‐azine‐4,7(5H,6H)diones have been prepared from the 3,4‐diacyl‐, 3‐carbethoxy‐4‐acyl‐, 3‐carbethoxy‐4‐cyano‐, and 3,4‐dicarbethoxy‐pyrazole derivatives and hydrazine hydrate. The structures of the compounds prepared were inferred from their elemental analyses and spectral data. On the basis of spectroscopic data it was concluded that pyrazolopyridazinones have the oxo form, whereas the monohydroxymono oxo structure is pref

ISSN:0022-152X    

DOI:10.1002/jhet.5570140303

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

AbstractA facile route for the synthesis of substituted 2‐amino‐3‐cyano‐4‐methylpyrroles fromN‐acetyl‐α‐amino ketones and malononit

ISSN:0022-152X    

DOI:10.1002/jhet.5570140304

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

AbstractThe structure of 1,4‐rlihydro[1 ]benzothiopyrano[4,3‐c ]pyrazole 5,5‐dioxide was determined by single crystal x‐ray diffraction. The molecule crystallizes in space group P21/c with a = 13.4378(6), b = 5.5938(3), c = 12.9837(6)Å, and β = 103.831°. The final R value is 0.083. Surprisingly, the tautomer with N(2)‐H exists in the crystal with the pyrazole ring being planar. The entire system is not planar as the benzene ring is rotated about C(9a) and C(9b) with respect to the pyrazole ring. In the crystal structure the pyrazole exists as hydrogen‐bonded dimers with two molecules related by a cent

ISSN:0022-152X    

DOI:10.1002/jhet.5570140305

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

AbstractPar action de l'acétylacétate d'éthyle ou de l'acétylacétone, sur des diamino‐4,5 pyrazoles, les pyrazolo[3,4‐b]diazépines‐1,4 sont synthétisées, soit directement, soit aprés cyclisation d'inter‐médiaires crotoniques ou cétoniques. Le sens de cyclisation et les structures des cycles diazépines sont démontrés. IIs correspondent á l'attaque initiale du carbonyle cétonique sur la fonct

ISSN:0022-152X    

DOI:10.1002/jhet.5570140306

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

AbstractDeux synthéses de bitriazoles caractérisé's par une jonution C3(5)‐N1′ ou N4‐N4′ sont rapportées et discutées. Elles font appel aux réactions de substitution nucléophile de I'halogene des halogénotriazoles par l'anion du triazole lui‐měme et aux réactions de désulfuration de bis‐s‐triazolothiadiazines par le Nickel Raney. La détermination de leur structure est prouvée par RMN. Les spectres UV de ces d

ISSN:0022-152X    

DOI:10.1002/jhet.5570140307

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

AbstractMass spectra of some twelve derivatives of 1,3,4‐thiadiazole are reported. The fragmentation scheme of the 1,3,4‐thiadiazole ring is specific and indicative as to the structure. Derivatives of 5‐phenyl‐1,3,4‐thiadiazoles show rearrangement to isothi

ISSN:0022-152X    

DOI:10.1002/jhet.5570140308

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

AbstractThe15N and13C nmr spectra of physostigmine are discussed along with complete assignment of the signals. This alkaloid15N nmr spectrum is notable because it contains nitrogens in three different environments.

ISSN:0022-152X    

DOI:10.1002/jhet.5570140309

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY

摘要:

Abstracts‐Triazolo[4,3‐b]pyridazine (I) reacted photochemieally with bieyélo[2.2.1]hepla‐2,5‐diene, 1,5‐cyclooctadiene, 1,3‐cyclooctadiene, methylene cyclohexane, diethyl cis‐1,2,3,6‐tetrahydro‐phthalate and ethyl 2‐cyclopentene‐1‐acetate to givt: the following products: theendoandexoisomers of 4a, 5, 8a, 9‐tetrahydro‐9‐rnethylene‐5,8‐rnethano‐8H‐s‐triuzolo[1, 5‐a]indole (II) and theendoandexo‐9‐cyanometliyl products (III and IV) from bicyclo[2.2.1] hepta‐2,5‐diene; 4a,5,‐9, 10, 10a, 11‐huxahydro‐11‐methylene‐6H‐cycloocta[4,5]pyrrolo[1,2‐b]‐s‐triazole (V) and the 11‐cyanomethyl product VI from 1,5‐cyclooctadiene: 4a,7,8,9,10,10a‐hexahydro‐11 ‐inethylene‐11H‐cycloocta[4,5]pyrrolo[1,2‐b]‐s‐triazole(VII),4a, 5, 7, 8, 10a, 11‐hexahydro‐11‐methylene‐6H‐cycloocta[4,5]pyrroIo[1,2‐b]‐s‐triazole (VIII) and their respective 9‐cyanomethyl products (X and 1X) from 1,3‐cyclooctadiene; 6′, 7′ ‐dihydro‐7′ ‐methylenespiro[cyclohexane‐1, 5′‐[5H] pyr‐rolo[1,2‐b]‐s‐triazole] (XI), 6′, 7′‐dihydro‐7′‐meth) lene. spiro cyclohexane‐1, 6′‐[5H]pyrrolo[1,2‐b]‐s‐triazole] (XII) and their respective 7 ‐eyanomethyl products (XIII and XIV) from melhylene cyclohexane; 6,7‐dicarbethoxy‐9‐cyanomelhyl‐4a, 5, 7, 8, 8a, 9‐hexahydro‐6H‐s‐triazolo[1,5‐a]indole (XV) from diethylcis‐1, 2, 3, 6‐tetrahydrophlhalate: and 5‐earl)elhoxymethyl‐8‐eyanomethyl‐4a, 5, 6, 7, 7a, 8‐hexahydrocyclopenta[4,5]pyrrolo( 1, 2‐b]‐s‐triazole (XVI) from ethyl 2, 2‐cyclo‐pentene‐1‐acetate. Many other alkenes, particularly the

ISSN:0022-152X    

DOI:10.1002/jhet.5570140310

出版商:Wiley‐Blackwell    

年代:1977

数据来源: WILEY