Ammonia → 1-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]4-amino-2(1H)-quinazolinone

HRID 365101노트

반응식

HRID 365101 반응식
[C:1]1([CH:7]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[C:20](=S)[NH:19][C:18]3=[O:28])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH3:35]>C(Cl)(Cl)Cl.CO>[C:1]1([CH:7]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[C:20]([NH2:35])=[N:19][C:18]3=[O:28])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 140145691-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]-4-thioxo-3,4-dihydro-2(1H)-quinazolinone

생성물 1

HCID 134883801-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]4-amino-2(1H)-quinazolinone

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6212Chloroform용매

실험 절차

A solution of 1-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]-4-thioxo-3,4-dihydro-2(1H)-quinazolinone (1.2 g) in chloroform (25 ml) and 20% ammonia in methanol (30 ml) was heated in an autoclave for 15 hours at 100° C. The reaction mixture was concentrated in vacuo and the residue was purified by subjecting to a column chromatography on silica gel using 5% methanol in chloroform for elution to give an oily residue. This oily residue was dissolved in methanol and this solution was acidified with conc.hydrochloric acid solution and then concentrated in vacuo to give a crystal of the object compound, which was recrystallized twice from a mixture of water and isoporpyl alcohol to give 1-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]-4-amino-2(1H)-quinazolinone.2HCl.H2O (0.6 g).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue was purified
  3. washby subjecting to a column chromatography on silica gel using 5% methanol in chloroform for elution
  4. customto give an oily residue
  5. concentrationhydrochloric acid solution and then concentrated in vacuo
  6. customto give a crystal of the object compound, which
  7. customwas recrystallized twice from a mixture of water and isoporpyl alcohol

출처 및 근거

ORD 기록
ord-d2af8eb63f5d4c74a91d904c31b56b03
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04608375

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