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Chlorosulfonic acid → 2,4,6-Trimethoxybenzene-1-sulfonyl chloride

HRID 1154144
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HRID 1154144 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[C:5]([O:11][CH3:12])[CH:4]=1.[Cl:13][S:14](O)(=[O:16])=[O:15]>ClCCl>[CH3:12][O:11][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([O:9][CH3:10])[C:6]=1[S:14]([Cl:13])(=[O:16])=[O:15]
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참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 693011,3,5-Trimethoxybenzene

생성물 1

HCID 159175192,4,6-Trimethoxybenzene-1-sulfonyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

In 500 ml of dichloromethane is dissolved 5.05 g of 1,3,5-trimethoxybenzene and the solution was cooled to -5°~-10° C. A solution of 6 ml of chlorosulfonic acid in 400 ml of dichloromethane was added dropwise, and the mixture was allowed to stand at room temperature. The reaction mixture was then treated as in Reference Example 1. The resulting product was crystallized from carbon tetrachloride and filtered. Yield 610 mg (6.3%), m.p. 126°-129° C.

후처리

  1. temperaturethe solution was cooled to -5°~-10° C
  2. customto stand at room temperature
  3. additionThe reaction mixture was then treated as in Reference Example 1
  4. customThe resulting product was crystallized from carbon tetrachloride
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-b3da34e3a0844fb0af586bf29621a65f
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04487726

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