2-Chloro-5-[4-(2-dimethylamino-ethyl)-piperazin-1-yl]-benzoic acid ethyl ester → 2-Chloro-5-[4-(2-dimethylaminoethyl)-piperazin-1-yl]-benzoic acid

HRID 2047364ノート

反応式

HRID 2047364 の反応式
C([O:3][C:4](=[O:23])[C:5]1[CH:10]=[C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][N:19]([CH3:21])[CH3:20])[CH2:13][CH2:12]2)[CH:8]=[CH:7][C:6]=1[Cl:22])C>CCO.[OH-].[Na+]>[Cl:22][C:6]1[CH:7]=[CH:8][C:9]([N:11]2[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][N:19]([CH3:21])[CH3:20])[CH2:15][CH2:16]2)=[CH:10][C:5]=1[C:4]([OH:23])=[O:3]

参加物

4

反応物 1

HCID 686703542-Chloro-5-[4-(2-dimethylamino-ethyl)-piperazin-1-yl]-benzoic acid ethyl ester

生成物 1

HCID 686700692-Chloro-5-[4-(2-dimethylaminoethyl)-piperazin-1-yl]-benzoic acid収率 58%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 2-chloro-5-[4-(2-dimethylamino-ethyl)-piperazin-1-yl]-benzoic acid ethyl ester (0.46 g, 1.36 mmol) in EtOH (6 mL) and NaOH 10% (2 mL) was heated at reflux overnight, then the reaction mixture was cooled to room temperature and the organic solvent concentrated by evaporation under reduced pressure. The resulting solution was neutralized by dropwise addition of 1N HCl and the water was then evaporated under reduced pressure. The resulting residue was dissolved in EtOH (10 mL), the insoluble material was filtered off and the filtrate concentrated under reduced pressure at room temperature, to obtain 0.24 g of the title compound (58%) without additional purification.

後処理

  1. temperatureat reflux overnight
  2. concentrationthe organic solvent concentrated by evaporation under reduced pressure
  3. additionThe resulting solution was neutralized by dropwise addition of 1N HCl
  4. customthe water was then evaporated under reduced pressure
  5. dissolutionThe resulting residue was dissolved in EtOH (10 mL)
  6. filtrationthe insoluble material was filtered off
  7. concentrationthe filtrate concentrated under reduced pressure at room temperature

出典と根拠

ORDレコード
ord-62e3c404776b437ba0e053aae2eda4b1
出典データセット
uspto-grants-2013_11
特許番号
US08592463B2

反応ノート

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