Phosphorus oxychloride → 2-Naphthalenesulfonyl chloride, 5-(acetylamino)-1-(acetyloxy)-

HRID 363973

반응식

HRID 363973 반응식
[C:1]([O:4][C:5]1[C:14]2[C:9](=[C:10]([NH:15][C:16]([CH3:18])=[O:17])[CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[S:19]([OH:22])(=O)=[O:20])(=[O:3])[CH3:2].S1(CCCC1)(=O)=O.P(Cl)(Cl)([Cl:32])=O>>[C:1]([O:4][C:5]1[C:14]2[C:9](=[C:10]([NH:15][C:16]([CH3:18])=[O:17])[CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[S:19]([Cl:32])(=[O:22])=[O:20])(=[O:3])[CH3:2]

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 31347SulfolaneHCID 1556985-Acetamido-1-(acetyloxy)naphthalene-2-sulfonic acid

생성물 1

HCID 941252-Naphthalenesulfonyl chloride, 5-(acetylamino)-1-(acetyloxy)-수율 81%

반응 조건

온도
40 °C

실험 절차

100 g of 1-acetoxy-5-acetaminonaphthalene-2-sulfonic acid was added to 500 ml of sulfolane, and 200 ml of phosphorus oxychloride was dropwise added thereto at 40° C. while stirring. After continuing stirring for about 1 hour, the reaction mixture was poured into 2 liters of ice water, and the precipitated crystals were collected by filtration, washed with water until the filtrate did not show acidity, and air-dried as such for 24 hours to obtain 70 g (81% yield) of product.

후처리

  1. additionwas dropwise added
  2. stirringAfter continuing stirring for about 1 hour
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed with water until the filtrate
  5. customair-dried as such for 24 hours

출처 및 근거

ORD 기록
ord-28785255badf43a0863ce38c95f228b8
출처 데이터셋
uspto-grants-1986_08
특허 번호
USH0000098

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