Potassium Carbonate → 6-Chloro-1,2-benzothiazole-3-carboxylic acid

HRID 424650ノート

反応式

HRID 424650 の反応式
[Mn]([O-])(=O)(=O)=O.[K+].[Cl:7][C:8]1[CH:18]=[CH:17][C:11]2[C:12]([CH2:15][OH:16])=[N:13][S:14][C:10]=2[CH:9]=1.C(=O)([O-])[O-:20].[K+].[K+]>O>[Cl:7][C:8]1[CH:18]=[CH:17][C:11]2[C:12]([C:15]([OH:20])=[O:16])=[N:13][S:14][C:10]=2[CH:9]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 516875Potassium PermanganateHCID 66703047HCID 66703047、化合物

生成物 1

HCID 534277106-Chloro-1,2-benzothiazole-3-carboxylic acid収率 15%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

Potassium permanganate (1.69 mmol) was added in several batches a solution of (6-chlorobenzo[d]isothiazol-3-yl)methanol (2.50 mmol) in water (3 mL). Potassium carbonate (2.90 mmol) was added and the reaction mixture was maintained for 30 min at 25° C. The insoluble materials were removed by filtration and the aqueous layer was extracted with ethyl acetate (3×10 mL). The pH of the aqueous layer was adjusted to 3-4 by the addition of 1 N hydrochloric acid and the reaction mixture was maintained for 10 min. The solids were collected by filtration to provide 6-chlorobenzo[d]isothiazole-3-carboxylic acid in 15% yield as a white solid.

後処理

  1. customThe insoluble materials were removed by filtration
  2. extractionthe aqueous layer was extracted with ethyl acetate (3×10 mL)
  3. additionThe pH of the aqueous layer was adjusted to 3-4 by the addition of 1 N hydrochloric acid
  4. temperaturethe reaction mixture was maintained for 10 min
  5. filtrationThe solids were collected by filtration

出典と根拠

ORDレコード
ord-56cab39ac54d463d948fdf52632f9ae2
出典データセット
uspto-grants-2012_01
特許番号
US08106066B2

反応ノート

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