1,4'-Bipiperidine → 3,5-Dimethyl-2-[4-[4-[2-(4-piperidinopiperidino)-ethoxy]benzoyl]benzylthio]-4(3H)-quinazolinone dihydrochloride

HRID 1291379노트

반응식

HRID 1291379 반응식
[Cl:1][CH2:2][CH2:3][O:4][C:5]1[CH:33]=[CH:32][C:8]([C:9]([C:11]2[CH:31]=[CH:30][C:14]([CH2:15][S:16][C:17]3[N:26]([CH3:27])[C:25](=[O:28])[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][C:23]=4[CH3:29])[N:18]=3)=[CH:13][CH:12]=2)=[O:10])=[CH:7][CH:6]=1.[N:34]1([CH:40]2[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]2)[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1>CN(C=O)C>[ClH:1].[ClH:1].[CH3:27][N:26]1[C:25](=[O:28])[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][C:23]=2[CH3:29])[N:18]=[C:17]1[S:16][CH2:15][C:14]1[CH:30]=[CH:31][C:11]([C:9](=[O:10])[C:8]2[CH:32]=[CH:33][C:5]([O:4][CH2:3][CH2:2][N:43]3[CH2:44][CH2:45][CH:40]([N:34]4[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]4)[CH2:41][CH2:42]3)=[CH:6][CH:7]=2)=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 786071,4'-BipiperidineHCID 189188132-[4-[4-(2-Chloroethoxy)benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

생성물 1

HCID 189192323,5-Dimethyl-2-[4-[4-[2-(4-piperidinopiperidino)-ethoxy]benzoyl]benzylthio]-4(3H)-quinazolinone dihydrochloride수율 137.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 2-[4-[4-(2-chloroethoxy)benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone (375 mg) and 4-piperidinopiperidine (434 mg) in DMF (5 ml) was stirred at 100° C. for 7 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, dried, and concentrated. Then, hydrogen chloride/ethyl acetate was added and the precipitated hydrochloride was recovered by filtration and dried to provide the title compound as colorless solid (368 mg).

후처리

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. additionThen, hydrogen chloride/ethyl acetate was added
  7. filtrationthe precipitated hydrochloride was recovered by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-449dd8d14ef349439cf551a2e47c5cf0
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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