tert-Butyl mercaptan → Ethyl 4-(tert-butylthio)-3-oxobutanoate
反応式
Cl[CH2:2][C:3](=[O:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH3:11][C:12]([SH:15])([CH3:14])[CH3:13].C(N(CC)CC)C>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C1COCC1>[CH2:8]([O:7][C:5](=[O:6])[CH2:4][C:3](=[O:10])[CH2:2][S:15][C:12]([CH3:14])([CH3:13])[CH3:11])[CH3:9]参加物
6
実験手順
Ethyl 4-chloroacetoacetate (7.5 mL, 51.9 mmol), 2-methyl-2-propanethiol (5.6 mL, 49.7 mmol), triethylamine (10.8 mL, 77.4 mmol), and catalytic tetrabutylammonium bromide were dissolved in THF (250 mL) and stirred at room temperature overnight. Silica gel was added, and the mixture was concentrated and filtered over a plug of silica gel to obtain the desired product (B-1), which was used without further purification.
後処理
- additionSilica gel was added
- concentrationthe mixture was concentrated
- filtrationfiltered over a plug of silica gel
出典と根拠
- ORDレコード
- ord-e4500a20d89a4aafa3a9db98fd3661f1
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841295B2
反応ノート
読み込み中…