1-Phenylpiperazine → 3-Methyl-2-[4-[4-(4-phenylpiperazinylmethyl)benzoyl]benzylthio]thieno[3,2-d]pyrimidin-4(3H)-one

HRID 1291346노트

반응식

HRID 1291346 반응식
[SH:1][C:2]1[N:3]([CH3:12])[C:4](=[O:11])[C:5]2[S:10][CH:9]=[CH:8][C:6]=2[N:7]=1.Br[CH2:14][C:15]1[CH:30]=[CH:29][C:18]([C:19]([C:21]2[CH:26]=[CH:25][C:24]([CH2:27]Br)=[CH:23][CH:22]=2)=[O:20])=[CH:17][CH:16]=1.[CH:31]1[CH:32]=[CH:33][C:34]([N:37]2[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)=[CH:35][CH:36]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:12][N:3]1[C:4](=[O:11])[C:5]2[S:10][CH:9]=[CH:8][C:6]=2[N:7]=[C:2]1[S:1][CH2:14][C:15]1[CH:30]=[CH:29][C:18]([C:19](=[O:20])[C:21]2[CH:26]=[CH:25][C:24]([CH2:27][N:40]3[CH2:41][CH2:42][N:37]([C:34]4[CH:35]=[CH:36][CH:31]=[CH:32][CH:33]=4)[CH2:38][CH2:39]3)=[CH:23][CH:22]=2)=[CH:17][CH:16]=1

참가 물질

6

반응물 4

HCID 70961-PhenylpiperazineHCID 11430Potassium CarbonateHCID 23039244,4'-Bis(bromomethyl)benzophenoneHCID 178481668HCID 178481668, 화합물

생성물 1

HCID 189192423-Methyl-2-[4-[4-(4-phenylpiperazinylmethyl)benzoyl]benzylthio]thieno[3,2-d]pyrimidin-4(3H)-one수율 15.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 2-mercapto-3-methylthieno[3,2-d]-pyrimidin-4(3H)-one (990 mg), 4,4'-bis (bromomethyl)benzophenone (1.75 g), phenylpiperazine (810 mg) and potassium carbonate (828 mg) in DMF (30 ml) was stirred at 60° C. for 2 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate. The solution was washed with water, dried, and concentrated, and the residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=250:1:0.1) to provide the title compound as light-yellow syrup (428 mg).

후처리

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe solution was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customthe residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=250:1:0.1)

출처 및 근거

ORD 기록
ord-da82c456386f405c9142af27998083c0
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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