Diethyl Ether → tert-Butyl-(3-chloromethylsulfanyl-phenoxy)-dimethyl-silane

HRID 1685666

반응식

HRID 1685666 반응식
C1CCN2C(=NCCC2)CC1.[C:12]([Si:16]([CH3:26])([CH3:25])[O:17][C:18]1[CH:19]=[C:20]([SH:24])[CH:21]=[CH:22][CH:23]=1)([CH3:15])([CH3:14])[CH3:13].CCOCC.OS([O-])(=O)=O.[K+].Br[CH2:39][Cl:40]>>[C:12]([Si:16]([O:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([S:24][CH2:39][Cl:40])[CH:19]=1)([CH3:26])[CH3:25])([CH3:15])([CH3:14])[CH3:13]

참가 물질

6

반응물 5

HCID 3283Diethyl EtherHCID 6333BromochloromethaneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 516920Potassium bisulfateHCID 219768683-[[(1,1-Dimethylethyl)dimethylsilyl]oxy]benzenethiol

생성물 1

HCID 58734012tert-Butyl-(3-chloromethylsulfanyl-phenoxy)-dimethyl-silane

실험 절차

DBU (914 mg, 6.0 mmol) was added to a solution of 3-(tert-Butyl-dimethyl-silanyloxy)-benzenethiol (1.00 g, 4.16 mmol) in bromo-chloro methane (5 ml) at room temperature. Stirring was continued for 2 hours and Et2O (50 ml) and 2M KHSO4 (30 ml) were added. The organic layer was separated, washed with 2M KHSO4 (30 ml) and brine (30 ml), dried (Na2SO4) and concentrated under reduced pressure. The resulting oil was analysed by 1H-NMR spectroscopy and was used without further purification. Yield: 1.01 g (84%).

후처리

  1. customThe organic layer was separated
  2. washwashed with 2M KHSO4 (30 ml) and brine (30 ml)
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated under reduced pressure
  5. customwas used without further purification

출처 및 근거

ORD 기록
ord-1507da1f180a4e8ea82054e9c26f141d
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148415B2

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