Tetrahydrofuran → [4-(Cyclopentyloxy)phenyl]methanamine
反応式
C1COCC1.[CH:6]1([O:11][C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[CH:14][CH:13]=2)[CH2:10][CH2:9][CH2:8][CH2:7]1>Cl>[CH:6]1([O:11][C:12]2[CH:13]=[CH:14][C:15]([CH2:16][NH2:17])=[CH:18][CH:19]=2)[CH2:7][CH2:8][CH2:9][CH2:10]1参加物
4
実験手順
Add a solution of 1M BH3-THF complex in THF (4.8 mL, 4.8 mmol) to neat 4-cyclopentyloxy-benzonitrile (300 mg, 1.6 mmol) and stir the mixture for 3 h at room temperature and then for 3 h at reflux. Cool to room temperature, pour the reaction into 2N aqueous HCl (10 mL) and stir the mixture for 1 h at room temperature then concentrate in vacuo. Dissolve the crude mixture in methanol and filter through SCX column eluting with methanol followed by 3M ammonia in methanol to obtain the title compound (223 mg, 73%).
後処理
- temperaturefor 3 h at reflux
- temperatureCool to room temperature
- additionpour
- stirringstir the mixture for 1 h at room temperature
- concentrationthen concentrate in vacuo
- dissolutionDissolve the crude mixture in methanol
- filtrationfilter through SCX column
- washeluting with methanol
出典と根拠
- ORDレコード
- ord-5dc61c6fbdb8470eb3457fc1ab1b7c8a
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08580780B2
反応ノート
読み込み中…