Water → Benzoic acid, 3-sulfo-

HRID 273914

반응식

HRID 273914 반응식
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3].ClS(C1C=CC=CC=1C(O)=O)(=O)=[O:16].O>C1(C)C(C)=CC=CC=1>[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])([OH:16])(=[O:4])=[O:3]

참가 물질

5

반응물 3

HCID 962WaterHCID 77641Benzoic acid, 3-(chlorosulfonyl)-HCID 144744642-(Chlorosulfonyl)benzoic acid

생성물 1

HCID 8477Benzoic acid, 3-sulfo-수율 95.6%

시약·촉매·용매 1

HCID 7237O-Xylene용매

반응 조건

온도
100 °C

실험 절차

300 g of 3-(chlorosulfonyl)benzoic acid containing 38.8% water (corresponding to 183.6 g (0.83 mol) of 100% chlorosulfonylbenzoic acid) are admixed with 150 g of water and heated at 100° C. for 1 hour. Then 600 g of xylene are added dropwise over 1 hour and a total of 260 ml of water are azeotropically distilled off with xylene. The reaction mixture is cooled and the precipitate is filtered off with suction. After drying at 100° C./100 torr (13.16 kPa) 164.7 g of 3-sulfobenzoic acid are obtained, the purity determined by titration being 97.7%; this corresponds to a yield of 95.6%.

후처리

  1. distillationa total of 260 ml of water are azeotropically distilled off with xylene
  2. temperatureThe reaction mixture is cooled
  3. filtrationthe precipitate is filtered off with suction
  4. dry with materialAfter drying at 100° C./100 torr (13.16 kPa) 164.7 g of 3-sulfobenzoic acid
  5. customare obtained

출처 및 근거

ORD 기록
ord-5c21ac4fce2b41ce973bccab5db1a867
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387711

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