tert-Butyl mercaptan → Ethyl 4-(tert-butylthio)-3-oxobutanoate

HRID 77497

반응식

HRID 77497 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

반응물 3

HCID 6387tert-Butyl mercaptanHCID 8471TriethylamineHCID 69484Ethyl 4-chloroacetoacetate

생성물 1

HCID 10465978Ethyl 4-(tert-butylthio)-3-oxobutanoate

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 8028Tetrahydrofuran용매

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

  1. additionSilica gel was added
  2. concentrationthe mixture was concentrated
  3. 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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