Potassium Carbonate → 2-(4-(4-Diphenylmethyl-piperazin-1-yl)-3-hydroxy-butyl]isoindolin-1,3-dione

HRID 1070756

반응식

HRID 1070756 반응식
[O:1]1[CH2:16][CH:2]1[CH2:3][CH2:4][N:5]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]1=[O:15].[CH:17]([N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[C:24]1([CH:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:30]2[CH2:31][CH2:32][N:33]([CH2:16][CH:2]([OH:1])[CH2:3][CH2:4][N:5]3[C:13](=[O:14])[C:12]4[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=4)[C:6]3=[O:15])[CH2:34][CH2:35]2)[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 70048BenzhydrylpiperazineHCID 3394332-[2-(oxiran-2-yl)ethyl]-2,3-dihydro-1H-isoindole-1,3-dione

생성물 1

HCID 223976852-(4-(4-Diphenylmethyl-piperazin-1-yl)-3-hydroxy-butyl]isoindolin-1,3-dione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5 g (˜25 mmol) 2-(3,4-epoxybutyl)-isoindolin-1,3-dione, 7.5 g (30 mmol) benzhydrylpiperazine and 3.5 g (25 mmol) potassium carbonate are stirred in DMF for 6 hours 80° C. After cooling, the reaction mixture is filtered and concentrated under vacuum. The residue is taken up in 300 ml acetic acid ethyl ester and washed three times each with 20 ml water. The organic phase is dried over sodium sulfate and the solvent is removed under vacuum. The residue is chromatographically purified over silica gel with CHCl3/CH3OH.

후처리

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture is filtered
  3. concentrationconcentrated under vacuum
  4. washwashed three times each with 20 ml water
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. customthe solvent is removed under vacuum
  7. customThe residue is chromatographically purified over silica gel with CHCl3/CH3OH

출처 및 근거

ORD 기록
ord-74029f5adc144f849d7c7dffec248640
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903118B1

연결된 노트

불러오는 중…