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Pyrrolidine → HCID 68692826、化合物

HRID 13775
ノート
印刷プレビュー

反応式

HRID 13775 の反応式
[CH2:1]([N:8]1[CH2:12][CH2:11][C@@H:10](OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH:24]1[CH2:28][CH2:27][CH2:26][CH2:25]1>C(O)C>[CH2:1]([N:8]1[CH2:12][CH2:11][C@H:10]([N:24]2[CH2:28][CH2:27][CH2:26][CH2:25]2)[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 31268PyrrolidineHCID 10471906Toluene-4-sulfonic acid (R)-1-benzyl-pyrrolidin-3-yl ester

生成物 1

HCID 68692826HCID 68692826、化合物収率 69.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
140 °C

実験手順

2.00 g of (R)-1-benzyl-3-(p-toluenesulfonyloxy)pyrrolidine (J. Med. Chem., 1992, 35, 4205-4208) was dissolved in 12 ml of ethanol, 1.63 g of pyrrolidine was added, and then the mixture was stirred at 140° C. for 20 hours in a sealed tube. The reaction solution was concentrated under reduced pressure, mixed with water, followed by extraction with ethyl acetate, and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain 0.97 g of the objective compound as a brown oily product.

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionmixed with water
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f30451cf738345dd942d1704a5674f1a
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07728131B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート