Methyl Isocyanate → HCID 20074957、化合物
反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH2:10][C:11]([O:13]C)=O)[NH2:9])=[CH:4][CH:3]=1.[CH3:15][N:16]=[C:17]=[O:18].C[O-].[Na+]>C(#N)C>[CH3:15][N:16]1[C:11](=[O:13])[CH2:10][N:8]([C:5]2[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][CH:6]=2)[NH:9][C:17]1=[O:18]参加物
5
実験手順
To a solution of methyl [1-(4-methylphenyl)hydrazino]acetate (2.25 g) in acetonitrile (10 ml) was added methyl isocyanate (2 ml) and the mixture was heated under reflux for 30 min. The solvent was removed in vacuo to give a solid which was treated with a solution of sodium methoxide (27 ml; from sodium (4 g) and methanol (200 ml)) according to the method of Example 3 to give a solid which was purified by trituration with System A (1:1) to give the title compound (1.51 g), m.p. 193°-194°, t.l.c. (ether) Rf 0.56.
後処理
- temperaturethe mixture was heated
- temperatureunder reflux for 30 min
- customThe solvent was removed in vacuo
- customto give a solid which
- customto give a solid which
- customwas purified by trituration with System A (1:1)
出典と根拠
- ORDレコード
- ord-8c5afcbe0a3c4fdebb882f9eaaa8a467
- 出典データセット
- uspto-grants-1991_01
- 特許番号
- US04985427
反応ノート
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