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Sodium borohydride → HCID 19434450、化合物

HRID 889033
ノート
印刷プレビュー

反応式

HRID 889033 の反応式
C([O:3][C:4]([CH:6]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=2)[C:7]1=[O:21])=O)C.[BH4-].[Na+]>C(O)C>[OH:3][CH2:4][CH:6]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:18])([F:19])[F:20])[CH:12]=2)[C:7]1=[O:21]
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 4311764Sodium borohydrideHCID 574296622-Oxo-1-(3-trifluoromethyl-phenyl)-pyrrolidine-3-carboxylic acid ethyl ester

生成物 1

HCID 19434450HCID 19434450、化合物収率 43%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
12.5 °C

実験手順

A mixture of 2-oxo-1-(3-trifluoromethyl-phenyl)-pyrrolidine-3-carboxylic acid ethyl ester obtained in step 2 (0.5 g, 1.6 mmol) and ethanol were cooled to 10-15° C. Sodium borohydride (0.126 g, 3.3 mmol) was added portion wise over a period of 20 min and the reaction mixture was stirred for 3.5 hrs at 20-25° C. The organic volatiles were evaporated and the residue was taken into brine solution (15 ml). The aqueous layer was extracted with ethyl acetate, dried over Na2SO4 and evaporated to obtain brown semi solid which was purified by preparative TLC to afford 3-Hydroxymethyl-1-(3-trifluoromethyl-phenyl)-pyrrolidin-2-one as a colorless oil (0.177 g, 43%).

後処理

  1. customThe organic volatiles were evaporated
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. dry with materialdried over Na2SO4
  4. customevaporated
  5. customto obtain brown semi solid which
  6. customwas purified by preparative TLC

出典と根拠

ORDレコード
ord-5ff374fc80a8489eb5aaf95d754e862a
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252797B2

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