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

HRID 654010

反応式

HRID 654010 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒2 回HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a33c0f384d364543b7c03887fdc98fb1
出典データセット
uspto-grants-1992_07
特許番号
US05130119

関連ノート

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