Water → Ethyl 4-(2,5-dichlorobenzyl)piperazine-1-carboxylate

HRID 649811

反応式

HRID 649811 の反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[Cl:18][C:19]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:20]=1[CH2:21]Cl.O>CN(C)C=O>[Cl:18][C:19]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:20]=1[CH2:21][N:9]1[CH2:8][CH2:7][N:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH2:11][CH2:10]1

参加物

6

反応物 4

HCID 962WaterHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 11430Potassium CarbonateHCID 759762,5-Dichlorobenzyl chloride

生成物 1

HCID 22458123Ethyl 4-(2,5-dichlorobenzyl)piperazine-1-carboxylate収率 63%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture comprising 1.94 g 1-ethoxycarbonylpiperazine and 3.45 g anhydrous potassium carbonate, in 20 mL of N,N-dimethylformamide, stirred at room temperature, under a nitrogen atmosphere, there was added 2.01 g of 2,5-dichlorobenzyl chloride. Then after 24 hr stirring at room temperature, this reaction mixture was poured into 200 mL of water, followed by extraction with ethyl acetate (3×100 mL). The obtained organic phase was dried over anhydrous sodium sulphate, followed by evaporation under vacuum. The obtained residue was then purified by flash chromatography (petroleum ether—ethyl acetate 85:15). The solvents were then evaporated off completely to give 2 g of Compound 14A (yield 63%).

後処理

  1. extractionfollowed by extraction with ethyl acetate (3×100 mL)
  2. dry with materialThe obtained organic phase was dried over anhydrous sodium sulphate
  3. customfollowed by evaporation under vacuum
  4. customThe obtained residue was then purified by flash chromatography (petroleum ether—ethyl acetate 85:15)
  5. customThe solvents were then evaporated off completely

出典と根拠

ORDレコード
ord-d159fbbd55bd4a90934b9504fd409427
出典データセット
uspto-grants-2001_08
特許番号
US06271234B1

関連ノート

読み込み中…