Ethanol → 1,4-Diethyl 2-formylbutanedioate

HRID 1088296

반응식

HRID 1088296 반응식
[CH2:1]([OH:3])C.[Na].[C:5]([O:14][CH2:15][CH3:16])(=[O:13])[CH2:6][CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].C(OCC)=O>C1(C)C=CC=CC=1.O>[CH:1]([CH:6]([CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])[C:5]([O:14][CH2:15][CH3:16])=[O:13])=[O:3]

참가 물질

7

반응물 4

HCID 702EthanolHCID 8025Ethyl formateHCID 31249Diethyl SuccinateHCID 5360545Sodium

생성물 1

HCID 2315001,4-Diethyl 2-formylbutanedioate

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

Ethanol (20 cm3) was added portionwise to a suspension of finely divided sodium (10.0 g) in dry toluene (100 cm3). On completion of the addition the mixture was heated for 3.5 hours at 80° C. To the resulting yellow suspension, cooled to 20° C., was added dropwise, over a period of 1 hour, a mixture of diethyl succinate (70.0 g) and ethyl formate (35.0 g), whilst the temperature of the mixture was maintained in the range 20° to 30° C. The mixture was kept at the ambient temperature for 16 hours after which water (100 cm3) was added carefully.

후처리

  1. additionOn completion of the addition the mixture
  2. temperatureTo the resulting yellow suspension, cooled to 20° C.
  3. additionwas added dropwise, over a period of 1 hour
  4. temperaturewhilst the temperature of the mixture was maintained in the range 20° to 30° C

출처 및 근거

ORD 기록
ord-f2be7aaf87b242a2a6134e8fe8001b38
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04962109

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