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Methanol → Methyl 3-(chlorosulfonyl)-1-benzothiophene-2-carboxylate

HRID 128257
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반응식

HRID 128257 반응식
Cl[C:2]([C:4]1[S:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[C:5]=1[S:13]([Cl:16])(=[O:15])=[O:14])=[O:3].[CH3:17][OH:18]>C(Cl)(Cl)Cl>[CH3:17][O:18][C:2]([C:4]1[S:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[C:5]=1[S:13]([Cl:16])(=[O:14])=[O:15])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 887MethanolHCID 536526182-Chlorocarbonyl-benzo[b]thiophene-3-sulfonic acid chloride

생성물 1

HCID 13178319Methyl 3-(chlorosulfonyl)-1-benzothiophene-2-carboxylate수율 53.5%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

168.0 gm (0.569 mol) of 2-chlorocarbonyl-benzo[b]thiophene-3-sulfonic acid chloride were dissolved in 1 liter of anhydrous chloroform, and the solution was admixed with 27.5 gm (0.858 mol) of dry methanol and refluxed for 3 hours. The reaction mixture was evaporated in vacuo, and the residue was recrystallized twice from a little methanol, yielding 88.5 gm (53.5% of theory) of colorless 2-methoxycarbonyl-benzo[b]-thiophene-3-sulfonic acid chloride. M.p.: 100°-101° C.

후처리

  1. temperaturerefluxed for 3 hours
  2. customThe reaction mixture was evaporated in vacuo
  3. customthe residue was recrystallized twice from a little methanol

출처 및 근거

ORD 기록
ord-00cedcb406b946fcbe4da1a8cf8c94cf
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04259336

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