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Acetonitrile → HCID 19007315, 화합물

HRID 1742688
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HRID 1742688 반응식
[C:1]([C:4]([CH:17]1[CH2:21][CH2:20][NH:19][CH2:18]1)([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)(=[O:3])[NH2:2].C(=O)([O-])[O-].[K+].[K+].[C:28](#[N:30])[CH3:29]>O>[C:1]([C:4]([CH:17]1[CH2:21][CH2:20][N:19]([CH2:18][CH2:17][C:4]2[CH:11]=[CH:12][C:29]([C:28]#[N:30])=[CH:6][CH:5]=2)[CH2:18]1)([C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)(=[O:3])[NH2:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 136337542,2-Diphenyl-2-(pyrrolidin-3-yl)acetamide

생성물 1

HCID 19007315HCID 19007315, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture contaiing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (0.6 g--g see Preparation 13), anhydrous potassium carbonate (0.5 g) and acetonitrile (20 ml) was heated under reflux for 1.5 hours. On cooling to room temperature, water (60 ml) was added and the mixture extracted with dichloromethane (3×50 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 6%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a colourless foam, yield, 0.25 g.

후처리

  1. temperatureunder reflux for 1.5 hours
  2. extractionthe mixture extracted with dichloromethane (3×50 ml)
  3. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customto give a gum which
  6. customwas purified by column chromatography on silica eluting with dichloromethane
  7. additioncontaining methanol (0% up to 6%)
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7a75c5b6a1b24daf82b4c05ea9f5fe17
출처 데이터셋
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05340831

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