Hydrochloric Acid → HCID 20827739、化合物

HRID 495622

反応式

HRID 495622 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][CH:14]=1)[CH2:5][NH:6][C:7](=[O:11])[O:8][CH2:9][CH3:10].Cl[C:16]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:19]([N+:25]([O-:27])=[O:26])=[CH:18][C:17]=1[C:28]([F:31])([F:30])[F:29].[H-].[Na+].Cl>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][CH:14]=1)[CH2:5][N:6]([C:16]1[C:17]([C:28]([F:30])([F:31])[F:29])=[CH:18][C:19]([N+:25]([O-:27])=[O:26])=[CH:20][C:21]=1[N+:22]([O-:24])=[O:23])[C:7](=[O:11])[O:8][CH2:9][CH3:10]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 67851Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)-HCID 17071127Ethyl [(3-chlorophenyl)methyl]carbamate

生成物 1

HCID 20827739HCID 20827739、化合物収率 9.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl 3-chlorobenzylcarbamate (720.3 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (829.1 mg) were dissolved in tetrahydrofuran (20 ml), and to the solution was added sodium hydride (147.1 mg). The reaction mixture was heated at reflux for 1.5 hours. After allowing to cool, to the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=10:1) to give the title compound (129.5 mg, 9%).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 1.5 hours
  3. temperatureto cool, to the reaction mixture
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-65ef8bcd7f7e4b638673690370d62ffb
出典データセット
uspto-grants-2005_09
特許番号
US06939887B2

関連ノート

読み込み中…