Lithium Hydroxide → [4-(3,3-diphenyl-propionyl)-piperazin-1-yl]-acetic Acid

HRID 456429ノート

反応式

HRID 456429 の反応式
C([O:3][C:4](=[O:28])[CH2:5][N:6]1[CH2:11][CH2:10][N:9]([C:12](=[O:27])[CH2:13][CH:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:8][CH2:7]1)C.[Li+].[OH-]>CO.O>[C:21]1([CH:14]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH2:13][C:12]([N:9]2[CH2:10][CH2:11][N:6]([CH2:5][C:4]([OH:28])=[O:3])[CH2:7][CH2:8]2)=[O:27])[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 58817810[4-(3,3-diphenyl-propionyl)-piperazin-1-yl]-acetic Acid Ethyl Ester

生成物 1

HCID 18437004[4-(3,3-diphenyl-propionyl)-piperazin-1-yl]-acetic Acid収率 78%

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

A mixture of [4-(3,3-diphenyl-propionyl)-piperazin-1-yl]-acetic acid ethyl ester (1.17 g, 3.07 mmol) and LiOH (645 mg, 15.35 mmol) in MeOH: H2O (3:1, 40 ml) stirred at room temperature for 2 days. The solvent was then evaporated and residue dissolved in water. Upon acidified with 2N HCl to pH 3, product precipitated in aq. phase, filtered and washed few times with water and dried to give the desired product in 78% yield.

後処理

  1. customThe solvent was then evaporated
  2. dissolutionresidue dissolved in water
  3. customprecipitated in aq. phase
  4. filtrationfiltered
  5. washwashed few times with water
  6. customdried

出典と根拠

ORDレコード
ord-ab4b2667b017452a9e359a6229a1bf05
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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