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Water → Diethyl 2-ethoxycarbonyloxyiminomalonate

HRID 1283751
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HRID 1283751 반응식
[OH:1][N:2]=[C:3]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5].O.Cl[C:16]([O:18][CH2:19][CH3:20])=[O:17].C(=O)([O-])O.[Na+]>CC(C)=O>[CH2:19]([O:18][C:16]([O:1][N:2]=[C:3]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5])=[O:17])[CH3:20]
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참가 물질

6

반응물 4

HCID 962WaterHCID 10928Ethyl chloroformateHCID 516892Sodium BicarbonateHCID 6399380Diethyl (hydroxyimino)malonate

생성물 1

HCID 20567995Diethyl 2-ethoxycarbonyloxyiminomalonate수율 101.7%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
0 °C

실험 절차

A mixture of diethyl 2-hydroxyiminomalonate (18.9 g), water (50 ml) and acetone (8 ml) is cooled at 0°C, and ethyl chloroformate (9.8 g) is dropwise added thereto. The resulting mixture is, after adjusted to pH 7 to 8 with the addition of an aqueous solution of sodium hydrogencarbonate, stirred at room temperature for 4 hours. The reaction mixture is extracted with ether, and the ether layer is washed with an aqueous solution of sodium chloride, dried and concentrated to give diethyl 2-ethoxycarbonyloxyiminomalonate (24 g) as an oil.

후처리

  1. extractionThe reaction mixture is extracted with ether
  2. washthe ether layer is washed with an aqueous solution of sodium chloride
  3. customdried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-03b5619f8c8840129fa6e04404648d1c
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03976635

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