Dimethylamine → 2-(3-aminooxetan-3-yl)-N,N-dimethylacetamide
反応式
[NH2:1][C:2]1([CH2:6][C:7]([O:9]CC)=O)[CH2:5][O:4][CH2:3]1.[CH3:12][NH:13][CH3:14].O>C1(C)C=CC=CC=1>[NH2:1][C:2]1([CH2:6][C:7]([N:13]([CH3:14])[CH3:12])=[O:9])[CH2:5][O:4][CH2:3]1参加物
5
実験手順
In a microwave tube was added ethyl 2-(3-aminooxetan-3-yl)acetate (CAN 1207175-54-9, 470 mg, 2.95 mmol). Toluene (7.0 ml) and 40%-dimethylamine solution in water (8.9 g, 10.0 ml, 79.0 mmol) were added. The tube was sealed and the reaction mixture was stirred vigorously at room temperature for 7 days. The reaction mixture was concentrated in vacuo and azeotroped several times with 30 mL toluene. The crude solid was dried under high vacuum at 40° C. for 3 hours to yield the title compound (405 mg, 87%). MS (ESI, m/z): 159.1 (M+H+).
後処理
- customThe tube was sealed
- concentrationThe reaction mixture was concentrated in vacuo
- customazeotroped several times with 30 mL toluene
- customThe crude solid was dried under high vacuum at 40° C. for 3 hours
出典と根拠
- ORDレコード
- ord-8f901fbe04b04054bb00ab8a33fa53f0
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09409866B2
反応ノート
読み込み中…