Water → [4-(3,3-diphenyl-propionyl)-piperazin-1-yl]-acetic Acid Ethyl Ester

HRID 456428ノート

反応式

HRID 456428 の反応式
[C:1]1([CH:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:8][C:9]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[CH2:28]([O:27][C:25](=[O:26])[CH2:24][N:14]1[CH2:13][CH2:12][N:11]([C:9](=[O:10])[CH2:8][CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:16][CH2:15]1)[CH3:29]

参加物

6

反応物 4

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 30301473,3-Diphenyl-1-(piperazin-1-yl)propan-1-one

生成物 1

HCID 58817810[4-(3,3-diphenyl-propionyl)-piperazin-1-yl]-acetic Acid Ethyl Ester収率 60%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

To a solution of 3,3-diphenyl-1-piperazin-1-yl-propan-1-one (2.0 g, 6.79 mmol) and ethyl bromoacetate (0.94 ml, 8.49 mmol) in dry DMF (15 ml) was added K2CO3 (2.7 g, 19.53 mmol) and the mixture was heated to 70° C. overnight. Reaction mixture was cooled and water (32 ml) was added. The product was extracted with ether, dried and evaporated. The residue was purified by column chromatography using hexane:ethyl acetate (1:4) to give the desired product in 60% yield.

後処理

  1. customReaction mixture
  2. temperaturewas cooled
  3. extractionThe product was extracted with ether
  4. customdried
  5. customevaporated
  6. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-50da0476aa054ee9a44d38c410468735
出典データセット
uspto-grants-2007_03
特許番号
US07186726B2

反応ノート

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