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Methanol → HCID 58728596, 화합물

HRID 1992230
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HRID 1992230 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([NH:12][S:13]([C:16]([F:19])([F:18])[F:17])(=[O:15])=[O:14])=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[OH-].[Na+].CO.O>Cl>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([NH:12][S:13]([C:16]([F:19])([F:17])[F:18])(=[O:14])=[O:15])=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 14798Sodium HydroxideHCID 58728461HCID 58728461, 화합물

생성물 1

HCID 58728596HCID 58728596, 화합물수율 82%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of methyl 2-chloro-5-{[(trifluoromethyl)sulfonyl]amino}benzoate (1.0 g, 3.15 mmol), sodium hydroxide (378 mg, 9.44 mmol), methanol (6 ml) and water (6 ml) was stirred for 1 hour. Removal of the volatiles by spin evaporation in vacuo gave a residue that was dissolved in 1 N aqueous hydrochloric acid. The aqueous solution was extracted with ethyl acetate (3 times) and the organic layers were combined, washed with water, and concentrated by spin evaporation in vacuo to give 2-chloro-5-{[(trifluoromethyl)sulfonyl]amino}benzoic acid as a crystalline solid (0.78 g, 82%). 1H-NMR (400 MHz, DMSO-d6): δ 7.63-7.60 (m, 1H), 7.59-7.54 (m, 1H), 7.40-7.35 (m, 1H). ES-LCMS m/z 304 (M+H).

후처리

  1. customRemoval of the volatiles
  2. customby spin evaporation in vacuo
  3. customgave a residue that
  4. extractionThe aqueous solution was extracted with ethyl acetate (3 times)
  5. washwashed with water
  6. concentrationconcentrated by spin evaporation in vacuo

출처 및 근거

ORD 기록
ord-13a7ec9a203541ddb5edf55cb88478ad
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645771B2

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