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3-methyl-3-Pentanol → HCID 86211537、化合物

HRID 2236010
ノート
印刷プレビュー

反応式

HRID 2236010 の反応式
[N:1]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[C:2]=[O:3].Cl.O1CCOCC1.[CH3:17][C:18]([OH:23])([CH2:21][CH3:22])[CH2:19][CH3:20]>ClCCl>[CH2:19]([C:18]([CH3:17])([O:23][C:2]([NH:1][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[O:3])[CH2:21][CH3:22])[CH3:20]
参加物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 64933-methyl-3-PentanolHCID 76283Ethyl isocyanatoacetateHCID 204431481,4-Dioxane hydrochloride

生成物 1

HCID 86211537HCID 86211537、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.500 ml (4.01 mmol) of ethyl isocyanatoacetate was dissolved in dichloromethane. 0.05 ml of 4 N hydrochloric acid/1,4-dioxane solution was added to the obtained solution, and they were stirred at room temperature for 5 minutes. 0.547 ml (4.41 mmol) of 3-methyl-3-pentanol was added to the reaction mixture, and they were stirred overnight. After the concentration under reduced pressure, ethyl acetate was added to the reaction mixture, and they were washed with saturated aqueous sodium hydrogencarbonate solution, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was washed with diethyl ether. The filtrate was concentrated under reduced pressure to obtain the title compound.

後処理

  1. stirringwere stirred overnight
  2. concentrationAfter the concentration under reduced pressure, ethyl acetate
  3. additionwas added to the reaction mixture, and they
  4. washwere washed with saturated aqueous sodium hydrogencarbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. washThe residue was washed with diethyl ether
  8. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-ee59025df9714bc4bcea3d8ded933b0d
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07713957B2

反応ノート

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