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

HRID 2390944노트

반응식

HRID 2390944 반응식
[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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 516875Potassium PermanganateHCID 66703047HCID 66703047, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e8432186807c4a83b3d36f5c2d9073fd
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273891B2

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