Hydrazine → Hydrazinecarboxylic acid, phenyl ester
反応式
[NH2:1][NH2:2].Cl[C:4]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:5]>CCOCC>[NH:1]([C:4]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:5])[NH2:2]参加物
4
実験手順
To a solution of hydrazine (0.83 mL, 26 mmol) in ether was added phenyl chloroformate (0.92 mL, 7.4 mmol) at −20° C. The solution was stirred for 1 h, removed solid by filtration, and filtrate was concentrated to give phenyl hydrazinecarboxylate. To phenyl hydrazinecarboxylate was added compound 2b (1.2 g, 5.2 mmol), THF (20 mL), and DIPEA (1.5 mL) and the solution was stirred for 1 h. Partitioned reaction between sat. aq. NaHCO3 and CH2Cl2, dried (MgSO4), filtered, and concentrated to yield compound 81a (400 mg, 22%).
後処理
- customremoved solid
- filtrationby filtration, and filtrate
- concentrationwas concentrated
出典と根拠
- ORDレコード
- ord-46c70f04a18b48ae8e42b25d80a6957d
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415353B2
反応ノート
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