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Sodium hydride → N-[4-(6-Fluorobenzothiazol-2-ylmethoxy)phenyl]acetamide

HRID 1597782
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HRID 1597782 반응식
[H-].[Na+].[F:3][C:4]1[CH:18]=[CH:17][C:7]2[N:8]=[C:9]([CH2:11][O:12]S(C)(=O)=O)[S:10][C:6]=2[CH:5]=1.[Cl-].[NH4+:20]>CN(C)C=O>[F:3][C:4]1[CH:18]=[CH:17][C:7]2[N:8]=[C:9]([CH2:11][O:12][C:4]3[CH:18]=[CH:17][C:7]([NH:20][C:11](=[O:12])[CH3:9])=[CH:6][CH:5]=3)[S:10][C:6]=2[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 189321066-Fluoro-2-methanesulfonyloxymethylbenzothiazole

생성물 1

HCID 18932502N-[4-(6-Fluorobenzothiazol-2-ylmethoxy)phenyl]acetamide수율 28%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

18.8 mg of sodium hydride (as a 60% w/w dispersion in mineral oil) were added to a solution of 64.6 mg of4-acetamidophenol in 1.3 ml of dimethylformamide cooled in an ice-water bath, and the resulting mixture stirred at the same temperature for 3 minutes. A solution of 122.8 mg of 6-fluoro-2-methanesulfonyloxymethylbenzothiazole [prepared as described in step (c) above] in 0.4 ml of dimethylformamide was then added to the reaction mixture. The temperature of the resulting mixture was then elevated to room temperature and the mixture was stirred for 3 hours. At the end of this time, a saturated aqueous ammonium chloride solution was added to the reaction mixture and the resulting mixture was extracted with ethyl acetate. The resulting extract was washed consecutively with water and an aqueous sodium chloride solution and then dried over sodium sulfate. The solvent was removed by evaporation under reduced pressure, and the resulting residue was purified by column chromatography through silica gel using a 1:2 by volume mixture of hexane and ethyl acetate as the eluent, to give 38.3 mg (yield 28%) of the title compound as a solid having a melting point of 204° to 205° C.

후처리

  1. temperaturecooled in an ice-water bath
  2. customwas then elevated to room temperature
  3. stirringthe mixture was stirred for 3 hours
  4. extractionthe resulting mixture was extracted with ethyl acetate
  5. extractionThe resulting extract
  6. washwas washed consecutively with water
  7. dry with materialan aqueous sodium chloride solution and then dried over sodium sulfate
  8. customThe solvent was removed by evaporation under reduced pressure
  9. customthe resulting residue was purified by column chromatography through silica gel using a 1:2
  10. additionby volume mixture of hexane and ethyl acetate as the eluent

출처 및 근거

ORD 기록
ord-8b530076007f4fdf86f8248b17acb2b8
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05736487

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