Dimethylamine → HCID 2762435、化合物
反応式
[CH3:1][NH:2][CH3:3].[CH2:4]=O.[CH3:6][C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[CH:9]=[CH:10][NH:11]2.[OH-].[Na+]>C(O)(=O)C>[CH3:1][N:2]([CH3:4])[CH2:3][C:9]1[C:8]2[C:12](=[CH:13][CH:14]=[CH:15][C:7]=2[CH3:6])[NH:11][CH:10]=1参加物
6
実験手順
To a chilled solution of dimethyl amine (30 mL, 40% in water, 120 mmol) and formalin (13 mL, 37% in water, 84 mmol) in glacial acetic acid (30 mL) is added 4-methyl indole (21 g, 165 mmol) at 0° C. The reaction is warmed to room temperature and stirred for 3 hours. The reaction mixture is brought to pH 12 by addition of 50% NaOH and ice, and the product extracted with methylene chloride. The organic layers are dried over Na2SO4 filtered and evaporated in vacuo to give the title compound that is used without further purification (33 g, 162 mmol, 98%) LC/MS (M++1): 205.7.
後処理
- extractionthe product extracted with methylene chloride
- dry with materialThe organic layers are dried over Na2SO4
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-5e9430295ee14861a44a981cdbca0c98
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969348B2
反応ノート
読み込み中…