Water → Benzoic acid, 3-sulfo-

HRID 273915

反応式

HRID 273915 の反応式
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]

参加物

5

反応物 3

HCID 962Water2 回HCID 77641Benzoic acid, 3-(chlorosulfonyl)-HCID 144744642-(Chlorosulfonyl)benzoic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-f331762fe48d4032a45a6428d40a8c32
出典データセット
uspto-grants-1995_02
特許番号
US05387711

関連ノート

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