Water → N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide

HRID 257024

反応式

HRID 257024 の反応式
[CH2:1]([S:3]([NH2:6])(=[O:5])=[O:4])[CH3:2].[H-].[Na+].Cl[C:10]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][C:13]([C:19]([F:22])([F:21])[F:20])=[CH:12][N:11]=1.O>O1CCCC1>[N+:16]([C:15]1[C:10]([NH:6][S:3]([CH2:1][CH3:2])(=[O:5])=[O:4])=[N:11][CH:12]=[C:13]([C:19]([F:22])([F:20])[F:21])[CH:14]=1)([O-:18])=[O:17]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 73702EthanesulfonamideHCID 47369502-Chloro-3-nitro-5-(trifluoromethyl)pyridine

生成物 1

HCID 10851681N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide収率 54.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3.1 g of ethanesulfonamide was dissolved in 50 ml of dry tetrahydrofuran, and 1.2 g of 60% sodium hydride was added thereto under cooling with ice. After completion of the addition, the mixture was reacted for one hour under reflux. After cooling, 5.0 g of 2-chloro-3-nitro-5-trifluoromethylpyridine was added thereto, and then the mixture was reacted for 7 hours under reflux. After completion of the reaction, the reaction product was poured into 200 ml of water. Undissolved materials in water were extracted with ethyl ether and removed. Then, the aqueous layer was weakly acidified with dilute hydrochloric acid. Precipitated crystals were collected by filtration and dried to obtain 3.6 g of N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide having a melting point of from 160° to 163° C.

後処理

  1. temperatureunder cooling with ice
  2. additionAfter completion of the addition
  3. customthe mixture was reacted for one hour
  4. temperatureunder reflux
  5. temperatureAfter cooling
  6. customthe mixture was reacted for 7 hours
  7. temperatureunder reflux
  8. customAfter completion of the reaction
  9. extractionUndissolved materials in water were extracted with ethyl ether
  10. customremoved
  11. customPrecipitated crystals
  12. filtrationwere collected by filtration
  13. customdried

出典と根拠

ORDレコード
ord-da25dd324d444ea195b905ca178bf557
出典データセット
uspto-grants-1993_11
特許番号
US05260320

関連ノート

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