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Acetonitrile → HCID 19007315、化合物

HRID 1742688
ノート
印刷プレビュー

反応式

HRID 1742688 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 19007315HCID 19007315、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7a75c5b6a1b24daf82b4c05ea9f5fe17
出典データセット
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05340831

反応ノート

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