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Sodium hydride → (R)-2-(4-Phenoxy-phenylsulfanylmethyl)-pyrrolidine-1-carboxylic acid tert-butyl ester

HRID 749977
ノート
印刷プレビュー

反応式

HRID 749977 の反応式
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([SH:14])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[C:17]([O:21][C:22]([N:24]1[CH2:28][CH2:27][CH2:26][C@@H:25]1[CH2:29]OS(C1C=CC(C)=CC=1)(=O)=O)=[O:23])([CH3:20])([CH3:19])[CH3:18]>CN(C=O)C>[C:17]([O:21][C:22]([N:24]1[CH2:28][CH2:27][CH2:26][C@@H:25]1[CH2:29][S:14][C:11]1[CH:12]=[CH:13][C:8]([O:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:9][CH:10]=1)=[O:23])([CH3:20])([CH3:18])[CH3:19]
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

5

反応物 3

HCID 24758Sodium hydrideHCID 27603544-PhenoxythiophenolHCID 11760051(R)-tert-Butyl 2-((tosyloxy)methyl)pyrrolidine-1-carboxylate

生成物 1

HCID 68997777(R)-2-(4-Phenoxy-phenylsulfanylmethyl)-pyrrolidine-1-carboxylic acid tert-butyl ester収率 71.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
2.5 °C

実験手順

To a solution of 4-phenoxy benzenethiol (200 mg, 0.988 mmol) in DMF (3 mL) at 0-5° C. was added 60% NaH (73 mg, 1.83 mmol) at 0-5° C. The reaction mixture was stirred at rt for 15 min at 0-5° C. A solution of (R)-2-(Toluene-4-sulfonyloxymethyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (357 mg, 1 mmol) in DMF (2 mL) was added to the above mixture at 0-5° C. The reaction mixture was warmed to it and then heated at 90° C. for 15 h. The mixture was concentrated, diluted with saturated aq NaHCO3 and extracted with ethyl acetate. The aqueous layer was re-extracted with ethylacetate. The combined organic layers were dried over anhy. MgSO4 and the solvent was removed in vacuo to obtain the crude mixture, which was purified by silica gel flash chromatography to obtain the title product (272 mg, 71%).

後処理

  1. temperatureThe reaction mixture was warmed to it
  2. temperatureheated at 90° C. for 15 h
  3. concentrationThe mixture was concentrated
  4. additiondiluted with saturated aq NaHCO3
  5. extractionextracted with ethyl acetate
  6. extractionThe aqueous layer was re-extracted with ethylacetate
  7. customThe combined organic layers were dried over anhy
  8. customMgSO4 and the solvent was removed in vacuo
  9. customto obtain the crude mixture, which
  10. customwas purified by silica gel flash chromatography

出典と根拠

ORDレコード
ord-a8b1dbe02c1f4bd88e12a800dda686cb
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07402684B2

反応ノート

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