Chlorosuccinimide → Tert-butyl(2-(5-chlorothiophen-2-yl)ethoxy)dimethylsilane

HRID 446383노트

반응식

HRID 446383 반응식
C1C(=O)N([Cl:8])C(=O)C1.[C:9]([Si:13]([CH3:23])([CH3:22])[O:14][CH2:15][CH2:16][C:17]1[S:18][CH:19]=[CH:20][CH:21]=1)([CH3:12])([CH3:11])[CH3:10]>C(Cl)(Cl)Cl.C(Cl)Cl>[C:9]([Si:13]([O:14][CH2:15][CH2:16][C:17]1[S:18][C:19]([Cl:8])=[CH:20][CH:21]=1)([CH3:23])[CH3:22])([CH3:10])([CH3:12])[CH3:11]

참가 물질

5

반응물 2

HCID 31398ChlorosuccinimideHCID 22503634Tert-butyldimethyl(2-(thiophen-2-YL)ethoxy)silane

생성물 1

HCID 57989349Tert-butyl(2-(5-chlorothiophen-2-yl)ethoxy)dimethylsilane

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

NCS (0.826 g) was added portionwise to a solution of tert-butyldimethyl(2-(thiophen-2-yl)ethoxy)silane [WO 2008096129] (1.5 g) in chloroform (50 mL) and the resulting mixture was heated at reflux for 3 days. The mixture was diluted with DCM (100 mL) and washed with saturated aqueous sodium bicarbonate (2×100 mL) and brine (100 mL), then dried over sodium sulphate, filtered and evaporated. The residue was purified by silica gel chromatography eluting with isohexane to give the subtitled compound as a clear oil. Yield 1.00 g.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 3 days
  3. washwashed with saturated aqueous sodium bicarbonate (2×100 mL) and brine (100 mL)
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by silica gel chromatography
  8. washeluting with isohexane

출처 및 근거

ORD 기록
ord-43ca3383236e41dc81573665ebdc55f8
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476265B2

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