Chloroacetyl chloride → HCID 21491380、化合物
反応式
[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[NH:10][CH2:9][CH2:8][CH2:7]2.[Cl:12][CH2:13][C:14](Cl)=[O:15].CCN(CC)CC>C(Cl)Cl>[Cl:12][CH2:13][C:14]([N:10]1[C:11]2[C:6](=[CH:5][CH:4]=[CH:3][C:2]=2[CH3:1])[CH2:7][CH2:8][CH2:9]1)=[O:15]参加物
5
実験手順
To a solution of 8-methyl-1,2,3,4-tetrahydroquinoline (1) (2.77 g, 18.8 mmol) in dry CH2Cl2 (50 mL) at 0° C. was added chloroacetyl chloride (1.80 mL, 22.6 mmol) followed by dropwise addition of Et3N (6.30 mL, 45.2 mmol). The reaction was stirred overnight under N2. The reaction mixture was then diluted with CH2Cl2 (50 mL), washed with water (2×15 mL), and saturated NaCl (15 mL). Dried over MgSO4, filtered, and concentrated to give compound 2 (3.7 g). This crude material was used in subsequent reactions without further purification.
後処理
- washwashed with water (2×15 mL), and saturated NaCl (15 mL)
- dry with materialDried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-7fb6809d696d45f38035b07d74a1765d
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08916550B2
反応ノート
読み込み中…