Potassium Carbonate → 4-(Ethylsulfanyl)-2,2,3,3-tetramethyl-2,3-dihydroazete

HRID 1534005노트

반응식

HRID 1534005 반응식
F[B-](F)(F)F.[CH2:6]([O+](CC)CC)[CH3:7].[CH3:13][C:14]1([CH3:21])[NH:17][C:16](=[S:18])[C:15]1([CH3:20])[CH3:19].C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl>[CH2:6]([S:18][C:16]1[C:15]([CH3:20])([CH3:19])[C:14]([CH3:21])([CH3:13])[N:17]=1)[CH3:7]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2723982Triethyloxonium tetrafluoroborateHCID 19911807HCID 19911807, 화합물

생성물 1

HCID 144723344-(Ethylsulfanyl)-2,2,3,3-tetramethyl-2,3-dihydroazete

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 10.5 ml of triethyloxonium tetrafluoroborate as a 1M solution in CH2Cl2, a solution of 1 g (7 mmol) of tetramethylazetidinethione in 3 ml of dry CH2Cl2 was added under an inert atmosphere. The mixture was stirred at room temperature for 1 hour and then reflux for 1 hour. After cooling, it was added dropwise to 10 mol of a 50% K2CO3 solution at -10° C. After filtration, the organic phase was separated out and immediately dried over MgSO4. Filtration was followed by removal of the solvent under vacuum and the oily residue was subjected to flash silica chromatography (pet. ether : ethyl acetate ; 8:2) to obtain the product as a colorless oil.

후처리

  1. temperaturereflux for 1 hour
  2. temperatureAfter cooling
  3. filtrationAfter filtration
  4. customthe organic phase was separated out
  5. dry with materialimmediately dried over MgSO4
  6. filtrationFiltration
  7. customwas followed by removal of the solvent under vacuum

출처 및 근거

ORD 기록
ord-55d18a17d9fa4f6d8b8421dd36768904
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05086170

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