Sodium Hydroxide → 1,4-Dibenzylpiperazine-2-carboxylic acid

HRID 1713491노트

반응식

HRID 1713491 반응식
Cl.Cl.[C:3]1([CH2:9][N:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:12][CH:11]2[C:23]([O:25]CC)=[O:24])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[OH-].[Na+]>C(O)C>[C:3]1([CH2:9][N:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH2:12][CH:11]2[C:23]([OH:25])=[O:24])[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68419710Ethyl 1,4-dibenzylpiperazine-2-carboxylate dihydrochloride

생성물 1

HCID 223242451,4-Dibenzylpiperazine-2-carboxylic acid수율 76%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To ethyl 1,4-bis(phenylmethyl)-2-piperazine carboxylate dihydrochloride (21 g, 52 mmol) were added ethanol (300 mL) and a 1 M aqueous sodium hydroxide solution (300 mL, 0.30 mmol), and the mixture was stirred at 80° C. for 3 hours. The reaction solution was concentrated, and then 1 M hydrochloric acid was added thereto until the pH was adjusted to 5. The reaction solution was extracted with ethyl acetate, dried over anhydrous sodium sulfate and concentrated under reduced pressure. To the resulting crystals was added diethyl ether, collected by filtration, and washed with diethyl ether to obtain the title compound (12 g, yield 76%).

후처리

  1. concentrationThe reaction solution was concentrated
  2. addition1 M hydrochloric acid was added
  3. extractionThe reaction solution was extracted with ethyl acetate
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionTo the resulting crystals was added diethyl ether
  7. filtrationcollected by filtration
  8. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-f04e8b7c5e5e44ffa385461a767067a2
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795267B2

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