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

HRID 365101ノート

反応式

HRID 365101 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d2af8eb63f5d4c74a91d904c31b56b03
出典データセット
uspto-grants-1986_08
特許番号
US04608375

反応ノート

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