Water → Benzoic acid, 3-sulfo-

HRID 273915

반응식

HRID 273915 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].O.ClS(C1C=CC=CC=1C(O)=O)(=O)=[O:17]>C1(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:17])(=[O:4])=[O:3]

참가 물질

5

반응물 3

HCID 962Water2회HCID 77641Benzoic acid, 3-(chlorosulfonyl)-HCID 144744642-(Chlorosulfonyl)benzoic acid

생성물 1

HCID 8477Benzoic acid, 3-sulfo-수율 95.4%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

300 g of 3-(chlorosulfonyl)benzoic acid containing 38.8% of water (corresponding to 183.6 g (0.83 mol) of 100% chlorosulfonylbenzoic acid) are admixed with 100 g of water and heated to 100° C. for 1 hour. Then 500 g of toluene are added dropwise over 1 hour and a total of 164 ml of water distilled off azeotropically with toluene. The reaction mixture is cooled and the precipitated product filtered off with suction. After drying at 100° C./100 torr (13.16 kPa) 163.5 g of 3-sulfobenzoic acid are obtained, the purity determined by titration being 98.2%; this corresponds to a yield of 95.4%.

후처리

  1. distillationa total of 164 ml of water distilled off azeotropically with toluene
  2. temperatureThe reaction mixture is cooled
  3. filtrationthe precipitated product filtered off with suction
  4. dry with materialAfter drying at 100° C./100 torr (13.16 kPa) 163.5 g of 3-sulfobenzoic acid
  5. customare obtained

출처 및 근거

ORD 기록
ord-f331762fe48d4032a45a6428d40a8c32
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387711

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