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Aluminium lithium hydride → tert-butyl N-[2-(3,5-difluorophenyl)-1-oxopropan-2-yl]carbamate

HRID 1615788
ノート
印刷プレビュー

反応式

HRID 1615788 の反応式
[C:1]([O:5][C:6]([NH:8][C:9]([C:18]1[CH:23]=[C:22]([F:24])[CH:21]=[C:20]([F:25])[CH:19]=1)([CH3:17])[C:10](OC(C)(C)C)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[C:1]([O:5][C:6](=[O:7])[NH:8][C:9]([C:18]1[CH:23]=[C:22]([F:24])[CH:21]=[C:20]([F:25])[CH:19]=1)([CH3:17])[CH:10]=[O:11])([CH3:2])([CH3:3])[CH3:4]
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 21226445Aluminium lithium hydrideHCID 66865158tert-Butyl 2-[(tert-butoxycarbonyl)amino]-2-(3,5-difluorophenyl)propanoate

生成物 1

HCID 86616399tert-butyl N-[2-(3,5-difluorophenyl)-1-oxopropan-2-yl]carbamate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

To a stirred solution of tert-butyl 2-[(tert-butoxycarbonyl)amino]-2-(3,5-difluorophenyl)propanoate (27.0 g, 76 mmol) in THF (350 mL) at −78° C. was added LiAlH4 (76 mL of a 1 M solution in THF, 76 mmol), dropwise. The reaction mixture was stirred at −78° C. for 3 h, then quenched with EtOAc (76 mL), then H2O (228 mL), then 1 N aqueous NaOH (76 mL), then EtOAc (228 mL). The reaction mixture was warmed to ambient temperature, stirred for 1 h, filtered, and extracted with EtOAc (2×450 mL). The organic extracts were dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was purified by silica gel chromatography, eluting with hexane:EtOAc—100:0 to 70:30, to give the title compound. MS: m/z=186 (M−CO2C4H7).

後処理

  1. customquenched with EtOAc (76 mL)
  2. temperatureThe reaction mixture was warmed to ambient temperature
  3. stirringstirred for 1 h
  4. filtrationfiltered
  5. extractionextracted with EtOAc (2×450 mL)
  6. dry with materialThe organic extracts were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude product was purified by silica gel chromatography
  10. washeluting with hexane

出典と根拠

ORDレコード
ord-047f63c27e534fdb85cf8d8e4e857448
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765759B2

反応ノート

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