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Hydrochloric Acid → HCID 2050653、化合物

HRID 492986
ノート
印刷プレビュー

反応式

HRID 492986 の反応式
C([O:3][C:4](=[O:20])[CH2:5][N:6]1[CH2:11][CH2:10][N:9]([C:12](=[O:19])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:8][CH2:7]1)C.[OH-].[Li+].Cl>CO.O>[C:12]([N:9]1[CH2:8][CH2:7][N:6]([CH2:5][C:4]([OH:20])=[O:3])[CH2:11][CH2:10]1)(=[O:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 46673126HCID 46673126、化合物

生成物 1

HCID 2050653HCID 2050653、化合物収率 116.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

(4-Benzoylpiperazin-1-yl)acetic acid ethyl ester (8.19 g) was dissolved in methanol (300 ml) and water (50 ml), and then lithium hydroxide (1.34 g) was added thereto while cooling in an ice water bath, followed by stirring for 10 min. The reaction mixture was warmed to room temperature and then the mixture was stirred for 24 hrs. 1 N Hydrochloric acid (55.9 ml) was added to the reaction mixture, and the reaction mixture was concentrated under reduced pressure. Ethanol (200 ml) was added to the residue. The mixture was passed through Celite to remove the precipitated insoluble material. The obtained filtrate was concentrated under reduced pressure to provide a crude product of (4-benzoylpiperazin-1-yl)acetic acid (8.6 g) as a white solid.

後処理

  1. temperaturewhile cooling in an ice water bath
  2. stirringthe mixture was stirred for 24 hrs
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. additionEthanol (200 ml) was added to the residue
  5. customto remove the precipitated insoluble material
  6. concentrationThe obtained filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-0ae7a5140cfc4acd805a478afbc79cbe
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531532B2

反応ノート

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