Water → HCID 10803034、化合物

HRID 257025

反応式

HRID 257025 の反応式
[CH3:1][S:2]([NH2:5])(=[O:4])=[O:3].[H-].[Na+].Cl[C:9]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][C:12]([C:18]([F:21])([F:20])[F:19])=[CH:11][N:10]=1.O>O1CCCC1>[N+:15]([C:14]1[C:9]([NH:5][S:2]([CH3:1])(=[O:4])=[O:3])=[N:10][CH:11]=[C:12]([C:18]([F:21])([F:19])[F:20])[CH:13]=1)([O-:17])=[O:16]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 72879MethanesulfonamideHCID 47369502-Chloro-3-nitro-5-(trifluoromethyl)pyridine

生成物 1

HCID 10803034HCID 10803034、化合物収率 65.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4.4 g of methanesulfonamide was dissolved in 70 ml of dry tetrahydrofuran, and 1.9 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, 7.0 g of 2-chloro-3-nitro-5-trifluoromethylpyridine was added thereto, and the mixture was reacted for 6 hours under reflux. After completion of the reaction, the reaction product was poured into 300 ml of water and washed with ethyl ether. Then, the aqueous layer was weakly acidified with dilute hydrochloric acid. Precipitated crystals were collected by filtration and dried to obtain 5.8 g of N-(3-nitro-5-trifluoromethyl-2-pyridyl)methanesulfonamide having a melting point of from 138° to 139° 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 6 hours
  7. temperatureunder reflux
  8. customAfter completion of the reaction
  9. washwashed with ethyl ether
  10. customPrecipitated crystals
  11. filtrationwere collected by filtration
  12. customdried

出典と根拠

ORDレコード
ord-c328a21511944f4aab1efc7a3f853101
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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