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W.L. Mosby, J. Chem. Soc. 1957, 3997-4003　邮箱：xzlhh1015@163.com。谢谢

回复人：tri,▲▲ (hahaha) 时间：2005-12-12 03:51:13 编辑

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Reactions of some 1,4-dicarbonyl systems with hydrazine. Mosby, W. L.. Am. Cyanamid Co., Bound Brook, NJ, Journal of the Chemical Society, Abstracts (1957), 3997-4003. CODEN: JCSAAZ ISSN: 0590-9791.

Abstract

3,4-Diacetylhexane-2,5-dione (I) reacts with excess N2H4.H2O (II) to give 3,3',5,5'-tetramethyldipyrazol-4-yl (III), m. 299-300°, while a single equiv. of II and I gave 3-(3,5-dimethylpyrazol-4-yl)-pentane-2,4-dione (IV), m. 134-40°. Di-Et diacetylsuccinate (V) and II gave di-Et 1,4-dihydro-3,6-dimethylpyridazine-4,5-dicarboxylate(VI), m. 70-1°, l 210, 243, and 318mm. I (l 226 and 271 mm) (19.8 g.) was added to 30 ml. 85% II, the mixt. was cooled, filtered, washed with ice H2O and clarified with C in hot MeOH giving III, l 233 mm. Derivs. of III were prepd.: dinitrate; N,N'-diacetyl, m. 123.5-5.0°; N,N'-dibenzoyl, m. 126-8.5°. A mixt. of II (0.6 ml.) 2.0 g. I, and 50 ml. boiling alc. was clarified with C and evapd. in vacuo to give IV, l 217 and 285 mm. Aq. FeCl3 and IV gave a deep red color. II (1.8 ml.) and 6.0 g. 3,4-diacetyl-2,5-dimethylfuran in 10 ml. alc. gave 1,4,5,7-tetramethylfuro[3,4-d]pyridazine, m. 144° (decompn.), l 235, 272, 337 mm, picrate, m. 173-4.6°. A mixt. of II (3.0 ml.) and 3.0 g. 3,4-diacetyl-4,5-dimethylfuran in 8 ml. HCONMe2 was refluxed 2 hrs., cooled, filtered, washed with alc., and dried to give 4-amino-1,4,5,7-tetramethylpyrrolo[3,4-d]pyridazine (VII), m. 294-5°, l 229, 278, and 342 mm; picrate, m. 189.5-91.0°. VII and its neutral solns. fluoresce blue under ultraviolet light, and its acid solns. are green blue. An HOAc soln. of VII reacts with aq. NaNO2 at 5° to give 1,4,5,7-tetramethyl-6H-pyrrolo[3,4-d]pyridazine, m. above 300° (decompn.), l 225, 282, and 346 mm. I, benzhydrazide, and HOAc gave on refluxing 3,4-diacetyl-1-benzamido-2,5-dimethylpyrrole (VIII), m. 194.7-7.0°, l 230 and 265-276 mm. A mixt. of 1.20 g. VIII, 30 ml. alc., and 0.50 ml. II was refluxed 4 hrs., cooled, and filtered giving 460 mg. dibenzoylhydrazine, m. 241-1.8°, and 440 mg. 6-benzamido-1,4,5,7-tetramethylpyrrolo[3,4-d]pyridazine, m. 303.5-305°, l 232-246, 256, and 378 mm. 3,3'-Dimethyl-5,5'-dioxo-4,4'-dipyrazolinyl (IX) was prepd. from VI by B.ovrddot.ulow's method [Ber. 37, 91(1904)], l 247 mm.
Dibenzoyl deriv. of IX m. 270.2-1.2°, l 230.5 and 270 mm; tetraacetyl deriv., m. 136-7.5°. The tetrabenzoyl deriv. of IX, m. 197-201°, cannot be prepd. by the Schotten-Baumann reaction, but is prepd. by reaction with BzCl in pyridine.

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Paper
Journal of the Chemical Society (Resumed), 1957, 3997 - 4003
DOI: 10.1039/JR9570003997
793. The reactions of some 1 : 4-dicarbonyl systems with hydrazine
W. L. Mosby

回复人：xzlhh,▲ (希望能在这里得到大家的帮助，获得长足的进步) 时间：2005-12-12 10:24:07 编辑	2楼
楼上的朋友能不能发份全文过来啊，发到邮箱xzlhh1015@163.com

回复人：erro,★ (药物合成…… 希望认识更多的朋友) 时间：2005-12-12 10:31:28 编辑	3楼
好了,到 http://free.ys168.com/?erro xzlhh目录下载吧

回复人：xzlhh,▲ (希望能在这里得到大家的帮助，获得长足的进步) 时间：2005-12-12 11:10:23 编辑	4楼
谢谢

得分人：tri-1,erro-3,

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