Potassium Carbonate → Tert-butyl 4-benzhydrylpiperazine-1-carboxylate

HRID 1457606

반응식

HRID 1457606 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Br[CH:15]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)P(N(C)C)(N(C)C)=O>O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 12679HexamethylphosphoramideHCID 143452tert-Butyl piperazine-1-carboxylateHCID 236603Bromodiphenylmethane

생성물 1

HCID 4935532Tert-butyl 4-benzhydrylpiperazine-1-carboxylate수율 70.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3.7 g of N-(tert-butoxycarbonyl)piperazine, 2.5 g of bromodiphenylmethane, 6.9 g of potassium carbonate and 20 ml of hexamethylphosphoramide was stirred at 40° to 50° C. for 4 hours. After cooling, water was added and the reaction mixture was extracted with diethyl ether. The exact was washed and dried, and the solvent was removed under reduced pressure. Hexane was added to the precipitated crystals and the crystals were collected by filtration to give 2.5 g of 4-(tert-butoxycarbonyl)-1-diphenylmethylpiperazine (melting point: 129°-131° C.).

후처리

  1. temperatureAfter cooling
  2. extractionthe reaction mixture was extracted with diethyl ether
  3. washThe exact was washed
  4. customdried
  5. customthe solvent was removed under reduced pressure
  6. additionHexane was added to the precipitated crystals
  7. filtrationthe crystals were collected by filtration

출처 및 근거

ORD 기록
ord-07f4804c63e542a694dcb1c822559c1c
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849732

연결된 노트

불러오는 중…