Acetic Acid → HCID 15017643、化合物
反応式
[CH3:1][N:2]([CH3:11])[C:3]1[S:4][CH:5]=[C:6]([CH2:8][CH2:9][NH2:10])[N:7]=1.C=O.[C:14](O)(=O)C>O.CO>[CH3:11][N:2]([CH3:1])[C:3]1[S:4][C:5]2[CH2:14][NH:10][CH2:9][CH2:8][C:6]=2[N:7]=1参加物
6
実験手順
2-Dimethylamino-4-(2-aminoethyl)thiazole (1.7 g, see preceding preparation), formaldehyde (0.78 ml of a 37% solution in water, 9.6 mmol) and acetic acid (0.15 ml, 2.6 mmol) were combined in methanol (100 ml). After 2.5 hours at room temperature, the reaction mixture was treated with additional formaldehyde (0.15 ml, 1.8 mmol) and allowed to stir for an additional 16 hours. The reaction was then filtered, and the filtrate was concentrated in vacuo and purified by column chromatography (eluant: 89:10:1 of chloroform:methanol:concentrated ammonium hydroxide), providing the title product as a white solid (1.04 g, 5.7 mmol).
後処理
- filtrationThe reaction was then filtered
- concentrationthe filtrate was concentrated in vacuo
- custompurified by column chromatography (eluant: 89:10:1 of chloroform:methanol:concentrated ammonium hydroxide)
出典と根拠
- ORDレコード
- ord-cba5fcd9d46d46cdb9c7eca0684ae0fa
- 出典データセット
- uspto-grants-1993_05
- 特許番号
- US05214051
反応ノート
読み込み中…