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

HRID 2061230
ノート
印刷プレビュー

反応式

HRID 2061230 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 sodium 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 sodium 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-116a8a984cf34a56ac9985fe05f815c0
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08278329B2

反応ノート

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