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Water → 2-Chloro-6-phenylbenzenesulfonamide

HRID 236230
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HRID 236230 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:3]=1[S:14]([NH:17]C(C)(C)C)(=[O:16])=[O:15].O>FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:3]=1[S:14]([NH2:17])(=[O:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 962WaterHCID 138523512-Chloro-N-(1,1-dimethylethyl)-6-phenylbenzenesulfonamide

생성물 1

HCID 138523522-Chloro-6-phenylbenzenesulfonamide수율 83.6%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 2-chloro-N-(1,1-dimethylethyl)-6-phenylbenzenesulfonamide (23 g, 0.071 mol) in a mixture of 120 ml trifluoroacetic acid (TFA) plus 4 ml water was heated to reflux for 2 hours. The TFA was evaporated in vacuo and the residue partitioned between methylene chloride and water. The organic layer was dried (MgSO4), evaporated, and the residue crystallized from ether/methylene chloride to afford 15.9 g of crystalline solid in two crops, m.p. 185°-87°. NMR (90 MHZ, CDCl3) 6.45 (s, br, NH2). 7.3-7.7 (m, 8H) ppm.

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후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. customThe TFA was evaporated in vacuo
  4. customthe residue partitioned between methylene chloride and water
  5. dry with materialThe organic layer was dried (MgSO4)
  6. customevaporated
  7. customthe residue crystallized from ether/methylene chloride

출처 및 근거

ORD 기록
ord-55d38d434a644a75b9e768c1bf1f5464
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04643761

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