Hydrochloric Acid → 1-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]-3-methyl-2,4(1H,3H)quinazolinedione

HRID 365103ノート

反応式

HRID 365103 の反応式
Br[CH2:2][CH2:3][CH2:4][N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8](=[O:15])[N:7]([CH3:16])[C:6]1=[O:17].[C:18]1([CH:24]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].Cl>CO.O.CN(C)C=O>[C:31]1([CH:24]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:25]2[CH2:26][CH2:27][N:28]([CH2:2][CH2:3][CH2:4][N:5]3[C:14]4[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=4)[C:8](=[O:15])[N:7]([CH3:16])[C:6]3=[O:17])[CH2:29][CH2:30]2)[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 70048BenzhydrylpiperazineHCID 136872081-(3-bromopropyl)-3-methyl-2,4(1H)-quinazolinedione

生成物 1

HCID 134883851-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]-3-methyl-2,4(1H,3H)quinazolinedione

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A mixture of 1-(3-bromopropyl)-3-methyl-2,4(1H,3H)-quinazolinedione (1.68 g), 1-diphenylmethylpiperazine (1.56 g), anhydrous potassium carbonate (2.33 g) and N,N-dimethylformamide (8 ml) was stirred for 3 hours at 60° C. After cooling, water was added to the reaction mixture and then the mixture was extracted twice with chloroform. The chloroform layer was washed with water and with saturated sodium chloride aqueous solution respectively, dried over anhydrous magnesium sulfate and evaporated in vacuo to give an oily residue. This oily residue was dissolved in methanol and then conc.hydrochloric acid solution was dropwise added to the solution to give a crystal, which was collected by filtration, washed with water and dried. This crude crystal was recrystallized from a mixture of methanol and water, to give 1-[3-{4-(diphenylmethyl)piperazin-1-yl}propyl]-3-methyl-2,4(1H,3H)quinazolinedione.2HCl.0.5H2O (2.4 g).

後処理

  1. temperatureAfter cooling
  2. extractionthe mixture was extracted twice with chloroform
  3. washThe chloroform layer was washed with water and with saturated sodium chloride aqueous solution respectively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated in vacuo
  6. customto give an oily residue
  7. customto give a crystal, which
  8. filtrationwas collected by filtration
  9. washwashed with water
  10. customdried
  11. customThis crude crystal was recrystallized from a mixture of methanol and water

出典と根拠

ORDレコード
ord-4df21c82b8664ed6b898e16aec93f1d1
出典データセット
uspto-grants-1986_08
特許番号
US04608375

反応ノート

読み込み中…