Potassium Carbonate → HCID 22741906、化合物

HRID 324737

反応式

HRID 324737 の反応式
Cl[C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].[CH3:16][N:17]1[CH2:22][CH2:21][CH2:20][CH:19]([C:23]2[CH:24]=[C:25]([CH:27]=[CH:28][CH:29]=2)[NH2:26])[CH2:18]1.C(=O)([O-])[O-].[K+].[K+]>>[CH3:16][N:17]1[CH2:22][CH2:21][CH2:20][CH:19]([C:23]2[CH:24]=[C:25]([NH:26][C:2]3[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]=3[N+:13]([O-:15])=[O:14])[CH:27]=[CH:28][CH:29]=2)[CH2:18]1

参加物

4

反応物 3

HCID 11430Potassium CarbonateHCID 1268247Ethyl 4-chloro-3-nitrobenzoateHCID 22741929HCID 22741929、化合物

生成物 1

HCID 22741906HCID 22741906、化合物収率 98%

反応条件

温度
70 °C

実験手順

A mixture of 1c (5.7 g, 25 mmol), 2j (3.8 g, 20 mmol) and potassium carbonate (3.45 g, 25 mmol) was heated to 70° C. under a stream of nitrogen. The resulting melt was stirred at 70° C. overnight. The reaction mixture was partitioned between water and ethyl acetate and the organic phase was extracted with diluted hydrochloric acid (4M). The aqueous phase was rendered alkaline by addition of aqueous sodium hydroxide (4M) and extracted with ethyl acetate. The organic phase was dried over sodium sulfate and the solvent was removed under reduced pressure to leave ethyl 4-(3-(1-methylpiperidin-3-yl)phenylamino)-3-nitrobenzoate (7.5 g, 98%) as an oil.

後処理

  1. customThe reaction mixture was partitioned between water and ethyl acetate
  2. extractionthe organic phase was extracted with diluted hydrochloric acid (4M)
  3. additionby addition of aqueous sodium hydroxide (4M)
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic phase was dried over sodium sulfate
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-1d471ddf64eb42a2b9b033a10de4e4a2
出典データセット
uspto-grants-2001_04
特許番号
US06218547B1

関連ノート

読み込み中…