Hydrochloric Acid → 2-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-acetic acid methyl ester

HRID 654010

반응식

HRID 654010 반응식
[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:3]=1.[CH3:13][O:14][C:15](=[O:21])[CH2:16][S:17](Cl)(=[O:19])=[O:18].Cl>N1C=CC=CC=1.ClCCl>[CH3:13][O:14][C:15](=[O:21])[CH2:16][S:17](=[O:19])(=[O:18])[NH:6][C:5]1[CH:7]=[CH:8][C:2]([F:1])=[CH:3][C:4]=1[C:9]([F:10])([F:11])[F:12]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 678534-Fluoro-2-(trifluoromethyl)anilineHCID 11435213Methyl (chlorosulfonyl)acetate

생성물 1

HCID 150576042-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-acetic acid methyl ester

시약·촉매·용매 2

HCID 1049Pyridine용매2회HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

5 g (27.64 mmol) of 4-fluoro-2-(trifluoromethyl)-aniline is dissolved in 25 ml of dry pyridine and the solution is cooled to 0° C. A solution of 4.82 g (27.4 mmol) of chlorosulfonyl acetic acid methyl ester in 20 ml of dichloromethane is instilled in the cooled solution in the course of about 10 minutes with the temperature being maintained. Then it is stirred for 6 hours at room temperature. The reaction solution is then diluted with 100 ml of dichloromethane, the pyridine is shaken out with 2N hydrochloric acid, the organic phase is dried on magnesium sulfate, filtered and evaporated to dryness. The residue is crystallized from diethyl ether/hexane yield is obtained as a crystallizate. Melting point 84°-86° C.

후처리

  1. customis instilled in the cooled solution in the course of about 10 minutes with the temperature
  2. temperaturebeing maintained
  3. customthe organic phase is dried on magnesium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe residue is crystallized from diethyl ether/hexane
  7. customyield
  8. customis obtained as a crystallizate

출처 및 근거

ORD 기록
ord-a33c0f384d364543b7c03887fdc98fb1
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05130119

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