Methanol → 5-Azaspiro[2.4]heptan-4-one, 7-amino-7-methyl-
反応式
Cl.Cl.[NH2:3][C:4]([C:8]1([C:11]([OH:13])=O)[CH2:10][CH2:9]1)([CH3:7])[CH2:5][NH2:6].C[Si](C)(C)N[Si](C)(C)C.CO>C(#N)C>[NH2:3][C:4]1([CH3:7])[C:8]2([CH2:10][CH2:9]2)[C:11](=[O:13])[NH:6][CH2:5]1参加物
5
反応条件
- 温度
- 100 °C
実験手順
To a solution (70 mL) of the crude 1-(1,2-diamino-1-methyl ethyl)-1-cyclopropanecarboxylic acid dihydrochloride (800 mg, 3.46 mmol) in acetonitrile was added 1,1,1,3,3,3-hexamethyldisilazane (7.38 mL, 34.6 mmol), and the mixture was heated under reflux in an oil bath at 100° C. for 4 hours under nitrogen atmosphere. The mixture was cooled to room temperature, and after adding methanol (70 mL), the solvent was removed by distillation under reduced pressure to obtain crude 7-amino-7-methyl-5-azaspiro[2.4]heptan-4-one as a pale brown gummy solid.
後処理
- temperaturethe mixture was heated
- temperatureThe mixture was cooled to room temperature
- customthe solvent was removed by distillation under reduced pressure
出典と根拠
- ORDレコード
- ord-d3bfa475a8c647819a60c833b3d551bf
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08476429B2
反応ノート
読み込み中…