Hydrazine → HCID 178497541、化合物
反応式
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH:11]=[CH:12][N:13](C)C)=[CH:6][C:5]=1[Cl:16].[NH2:18]N>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][NH:13][N:18]=2)=[CH:6][C:5]=1[Cl:16]参加物
4
実験手順
A solution of 2-chloro-4-(3-dimethylamino-2-propen-1-yl)-benzoic acid methyl ester of Step B (6.13 g, 22.9 mmol) and anhydrous hydrazine (1.44 mL, 45.8 mmol) in 15 mL of glacial acetic acid was heated at 90° C. for 30 minutes. The reaction mixture was concentrated in vacuo and the residue partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over sodium sulfate. The solvent was evaporated and the residual solid triturated with diethyl ether-hexane to give the title compound (5.1 g) as an orange solid.
後処理
- concentrationThe reaction mixture was concentrated in vacuo
- customthe residue partitioned between ethyl acetate and water
- washThe organic layer was washed with water and brine
- dry with materialdried over sodium sulfate
- customThe solvent was evaporated
- customthe residual solid triturated with diethyl ether-hexane
出典と根拠
- ORDレコード
- ord-1fa6c5236a814e8faa386d789bf0bc95
- 出典データセット
- uspto-grants-2001_05
- 特許番号
- US06235900B1
反応ノート
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