Water → HCID 68760855、化合物

HRID 494389

反応式

HRID 494389 の反応式
[H-].[Na+].[C:3]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])(=[O:9])[CH2:4][C:5]([O:7][CH3:8])=[O:6].Cl[C:16]1[CH:17]=[CH:18][C:19]([N+:27]([O-:29])=[O:28])=[C:20]([CH:26]=1)[C:21]([N:23]([CH3:25])[CH3:24])=[O:22].O>CN(C)C=O>[CH3:8][O:7][C:5](=[O:6])[CH:4]([C:16]1[CH:17]=[CH:18][C:19]([N+:27]([O-:29])=[O:28])=[C:20]([C:21](=[O:22])[N:23]([CH3:24])[CH3:25])[CH:26]=1)[C:3]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 2733872tert-Butyl methyl malonateHCID 229348075-Chloro-N,N-dimethyl-2-nitrobenzamide

生成物 1

HCID 68760855HCID 68760855、化合物収率 80.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

Sodium hydride (350 mg) was dissolved in dimethylformamide (10 mL)), and the solution was cooled to 0° C. After addition of tert-butyl methyl malonate (1.52 g), the mixture was stirred for one hour, and the 5-chloro-N,N-dimethyl-2-nitrobenzamide (1.0 g) obtained in Example 2a) was added thereto. The mixture was stirred at 70° C. for 4.5 hours and water was added thereto. The resulting solution was concentrated, diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate and purified by column chromatography on silica gel with ethyl acetate:hexane=1:1 to give the title compound (1.29 g).

後処理

  1. stirringThe mixture was stirred at 70° C. for 4.5 hours
  2. concentrationThe resulting solution was concentrated
  3. additiondiluted with ethyl acetate
  4. washwashed with water
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. custompurified by column chromatography on silica gel with ethyl acetate

出典と根拠

ORDレコード
ord-e35f076fe60b47d98db6c6cc01f6b664
出典データセット
uspto-grants-2009_05
特許番号
US07538140B2

関連ノート

読み込み中…