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HCID 86590764、化合物 → Tert-butyl {2-[3-(pyridin-3-yl)propoxy]ethyl}carbamate

HRID 1008050
ノート
印刷プレビュー

反応式

HRID 1008050 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]#[C:8][CH2:9][O:10][CH2:11][CH2:12][NH:13][C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[CH:2]=1>CO>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][CH2:8][CH2:9][O:10][CH2:11][CH2:12][NH:13][C:14](=[O:20])[O:15][C:16]([CH3:18])([CH3:17])[CH3:19])[CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 86590764HCID 86590764、化合物

生成物 1

HCID 85898855Tert-butyl {2-[3-(pyridin-3-yl)propoxy]ethyl}carbamate収率 92.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Under a nitrogen purge, 10% palladium on carbon (5.0 g) and 2-propanol (20 mL) were added to a pressure vessel. A solution of tert-butyl {2-[3-(pyridin-3-yl)prop-2-ynyloxy]ethyl}carbamate (22.7 g, 82.1 mmol) in methanol (200 mL) were then added. The vessel was purged three times with nitrogen and then placed under hydrogen pressure (50 psi, 3.4×105 Pa) for five hours. The reaction mixture was filtered through a layer of CELITE filter aid, and the filtrate was concentrated under reduced pressure to yield 21.3 g of tert-butyl {2-[3-(pyridin-3-yl)propoxy]ethyl}carbamate as a brown oil.

後処理

  1. customUnder a nitrogen purge
  • addition10% palladium on carbon (5.0 g) and 2-propanol (20 mL) were added to a pressure vessel
  • customThe vessel was purged three times with nitrogen
  • customfor five hours
  • filtrationThe reaction mixture was filtered through a layer of CELITE
  • filtrationfilter aid
  • concentrationthe filtrate was concentrated under reduced pressure
  • 出典と根拠

    ORDレコード
    ord-465eaaf7ca294ae5b9b07240121b8716
    出典データセット
    uspto-grants-2004_09
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US06797718B2

    反応ノート

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