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Water → Tert-butyl [2-(2-cyanoethoxy)ethyl]carbamate

HRID 410983
ノート
印刷プレビュー

反応式

HRID 410983 の反応式
[C:1]([O:5][C:6](=[O:11])[NH:7][CH2:8][CH2:9][OH:10])([CH3:4])([CH3:3])[CH3:2].C(OCC)(=O)C.O.[C:19](#[N:22])[CH:20]=[CH2:21]>>[C:1]([O:5][C:6](=[O:11])[NH:7][CH2:8][CH2:9][O:10][CH2:21][CH2:20][C:19]#[N:22])([CH3:4])([CH3:2])[CH3:3]
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 4

HCID 962WaterHCID 7855AcrylonitrileHCID 8857Ethyl AcetateHCID 2733206tert-butyl N-(2-hydroxyethyl)carbamate

生成物 1

HCID 85735740Tert-butyl [2-(2-cyanoethoxy)ethyl]carbamate

反応条件

温度
50 °C

実験手順

[2-(2-Cyano-ethoxy)-ethyl]-carbamic acid tert-butyl ester (430 mg) was prepared starting from (2-hydroxy-ethyl)-carbamic acid tert-butyl ester (320 mg) in acrylonitrile (1.5 mL). The reaction was heated to 50° C. for 1 h. The reaction was added to ethyl acetate (20 mL) and water (20 mL). The phases were separated and the aqueous phase was extracted twice with ethyl acetate. The combined organics were dried over sodium sulfate and then filtered. The solvent was evaporated and crude compound was purified by flash chromatography using hexane:ethyl actetate gradient.

後処理

  1. customThe phases were separated
  2. extractionthe aqueous phase was extracted twice with ethyl acetate
  3. dry with materialThe combined organics were dried over sodium sulfate
  4. filtrationfiltered
  5. customThe solvent was evaporated
  6. customcrude compound was purified by flash chromatography

出典と根拠

ORDレコード
ord-a94ddfcfea13446c80c4efd454500b28
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08759535B2

反応ノート

読み込み中…

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