Hydrochloric Acid → 7-[(2-Chlorobenzyl)oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

HRID 1169451노트

반응식

HRID 1169451 반응식
[Cl:1][C:2]1[CH:26]=[CH:25][CH:24]=[CH:23][C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]2[S:15](=[O:17])(=[O:16])[CH2:14][CH2:13][C:12]([C:18]([O:20]C)=[O:19])=[CH:11][C:10]=2[CH:22]=1.C(=O)([O-])[O-].[K+].[K+].Cl>C1COCC1.CO>[Cl:1][C:2]1[CH:26]=[CH:25][CH:24]=[CH:23][C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]2[S:15](=[O:17])(=[O:16])[CH2:14][CH2:13][C:12]([C:18]([OH:20])=[O:19])=[CH:11][C:10]=2[CH:22]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 22990149Methyl 7-[(2-chlorobenzyl)oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 229901167-[(2-Chlorobenzyl)oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid수율 89.8%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

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온도
65 °C

실험 절차

Into a solution of methyl 7-[(2-chlorobenzyl)oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (350 mg) in THF-methanol (7-3.5 ml) was added at room temperature a 2 M aqueous solution of potassium carbonate (0.9 mg), and the resulting mixture was stirred at 65° C. for 20 hours. After cooling to room temperature, the reaction mixture was mixed with 1 N hydrochloric acid (10 ml) and was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated solution of sodium chloride and was dried with magnesium sulfate. After concentration under reduced pressure, the precipitated crystals were collected by filtration. The crystals were washed with diisopropyl ether to obtain 7-[(2-chlorobenzyl)oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (303 mg) as colorless crystals.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionwas extracted with ethyl acetate
  3. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
  4. dry with materialwas dried with magnesium sulfate
  5. concentrationAfter concentration under reduced pressure
  6. filtrationthe precipitated crystals were collected by filtration
  7. washThe crystals were washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-36320599eb03470fad06c2795e004406
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627651B1

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