Water → Benzoic acid, 3-sulfo-

HRID 273914

反応式

HRID 273914 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].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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
100 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-5c21ac4fce2b41ce973bccab5db1a867
出典データセット
uspto-grants-1995_02
特許番号
US05387711

関連ノート

読み込み中…