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

HRID 2370401

반응식

HRID 2370401 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-5d019a5332e340b0aa2c8d0d059829c0
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710081B2

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