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Methanesulfonyl chloride → HCID 58591583, 화합물

HRID 746600
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HRID 746600 반응식
[S:1]1[C:5]([CH2:6][CH2:7][OH:8])=[CH:4][C:3]2[CH:9]=[CH:10][CH:11]=[CH:12][C:2]1=2.CCN(C(C)C)C(C)C.[S:22](Cl)([CH3:25])(=[O:24])=[O:23]>C(Cl)Cl>[S:1]1[C:5]([CH2:6][CH2:7][O:8][S:22]([CH3:25])(=[O:24])=[O:23])=[CH:4][C:3]2[CH:9]=[CH:10][CH:11]=[CH:12][C:2]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 280609Benzo(b)thiophene-2-ethanol

생성물 1

HCID 58591583HCID 58591583, 화합물수율 99.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 2-benzo[b]thiophen-2-yl-ethanol (16.8 mmol) in CH2Cl2 (60 mL) were added DIPEA (33.6 mmol) and mesylchloride (20.2 mmol.) The mixture was stirred for 18 hrs at RT, diluted with CH2Cl2, washed with sat. NaHCO3 (3×), brine (1×), dried (MgSO4) and concentrated in vacuo to give 4.3 g (99%) of methanesulfonic acid 2-benzo[b]thiophen-2-yl-ethyl ester which was used in the next step without further purification.

후처리

  1. washwashed with sat. NaHCO3 (3×), brine (1×)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-77cb905d7f5a41b199e7785654f7949e
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07393865B2

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