tert-Butyl mercaptan → Ethyl 4-(tert-butylthio)-3-oxobutanoate
반응식
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]참가 물질
6
실험 절차
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.
후처리
- additionSilica gel was added
- concentrationthe mixture was concentrated
- filtrationfiltered over a plug of silica gel
출처 및 근거
- ORD 기록
- ord-e4500a20d89a4aafa3a9db98fd3661f1
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08841295B2
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