Chlorosulfonic acid → 5-(Chlorosulfonyl)-2-(trifluoromethoxy)benzoic acid

HRID 1820720ノート

反応式

HRID 1820720 の反応式
[F:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:12]=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7].[Cl:15][S:16](O)(=[O:18])=[O:17]>>[Cl:15][S:16]([C:10]1[CH:11]=[CH:12][C:4]([O:3][C:2]([F:13])([F:14])[F:1])=[C:5]([CH:9]=1)[C:6]([OH:8])=[O:7])(=[O:18])=[O:17]

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 27772232-(Trifluoromethoxy)benzoic acid

生成物 1

HCID 866007055-(Chlorosulfonyl)-2-(trifluoromethoxy)benzoic acid

反応条件

温度
70 °C

実験手順

A solution of 2-trifluoromethoxy benzoic acid [1979-29-9] (1.0 g) was added in small batches to chlorosulfonic acid (3.2 mL) at 0° C. After completion of the addition, the reaction mixture was stirred at 70° C. for 4 hours then left at room temperature overnight and heated at 75° C. for another 3 hours. After such time the reaction was slowly poured onto ice, and the precipitate was then filtered, washed with water and dried to yield the title compound as a white solid (1.2 g). MS (m/e): 303.3 (M−H, 100%).

後処理

  1. additionAfter completion of the addition
  2. waitthen left at room temperature overnight
  3. temperatureheated at 75° C. for another 3 hours
  4. additionAfter such time the reaction was slowly poured onto ice
  5. filtrationthe precipitate was then filtered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-31a390aa208d44f4ad4293b0b98bfecd
出典データセット
uspto-grants-2009_10
特許番号
US07605163B2

反応ノート

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