Hydrochloric Acid → (2S,5R)-1-benzyl-2,5-dimethylpiperazine dihydrochloride

HRID 1978383노트

반응식

HRID 1978383 반응식
C(OC([N:8]1[CH2:13][C@@H:12]([CH3:14])[N:11]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:10][C@@H:9]1[CH3:22])=O)(C)(C)C.[ClH:23]>>[ClH:23].[ClH:23].[CH2:15]([N:11]1[CH2:10][C@@H:9]([CH3:22])[NH:8][CH2:13][C@@H:12]1[CH3:14])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 66598992(2S,5R)-4-Benzyl-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 44828683(2S,5R)-1-benzyl-2,5-dimethylpiperazine dihydrochloride

실험 절차

To 9.76 g (32.06 mmol.) of trans-1-tert-butoxycarbonyl-2,5-dimethyl-4-benzyl piperazine was added, at room temperature, 10 ml (120 mmol.) of 12N hydrochloric acid. The mixture was stirred for one hour. The solvent was distilled off under reduced pressure. To the residue was added 2-propanol, which was further concentrated. To the concentrate was added diethyl ether. The resulting crystals were collected by filtration and washed with 2-propanol and diethyl ether to give the object compound as white crystals. The yield was 7.97 g (90%).

후처리

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionTo the residue was added 2-propanol, which
  3. concentrationwas further concentrated
  4. additionTo the concentrate was added diethyl ether
  5. filtrationThe resulting crystals were collected by filtration
  6. washwashed with 2-propanol and diethyl ether

출처 및 근거

ORD 기록
ord-545d8013a24b4db088d42d84906a93cd
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235731B1

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