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Diethyl Malonate → HCID 54455773, 화합물

HRID 1388134
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HRID 1388134 반응식
[CH2:1]([O:3][C:4](=[O:11])[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].CC[O-].[Na+].[Na].[CH:17]1([O:23][CH2:24][CH2:25][CH2:26][CH2:27]Br)[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1>C(O)C>[CH2:1]([O:3][C:4](=[O:11])[CH:5]([CH2:27][CH2:26][CH2:25][CH2:24][O:23][CH:17]1[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7761Diethyl MalonateHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 20214109(4-Bromobutoxy)cyclohexane

생성물 1

HCID 54455773HCID 54455773, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

15 g of malonic acid diethyl ester are added dropwise at 50° C. to a solution of sodium ethylate, freshly prepared from 1.5 g of sodium and 30 ml of ethanol. This temperature is maintained for 1 hour and 11.7 g of 4-cyclohexyloxybutyl bromide are then added dropwise. When the addition is complete, the mixture is stirred for 3 hours at 60° C. and is concentrated considerably, 100 ml of ice water are added to the residue and the mixture is extracted 3 times with a total of 150 ml of methylene chloride. The combined organic phases are dried over sodium sulphate and the solvent is removed by distillation in vacuo, together with excess malonic acid diethyl ester. This gives 10.5 g of [4-(cyclohexyloxy)-butyl]-malonic acid diethyl ester in the form of a pale yellow oily residue.

후처리

  1. temperatureThis temperature is maintained for 1 hour
  2. additionWhen the addition
  3. concentrationis concentrated considerably
  4. addition100 ml of ice water are added to the residue
  5. extractionthe mixture is extracted 3 times with a total of 150 ml of methylene chloride
  6. dry with materialThe combined organic phases are dried over sodium sulphate
  7. customthe solvent is removed by distillation in vacuo, together with excess malonic acid diethyl ester

출처 및 근거

ORD 기록
ord-ba2bec645f404b4e94b7563d177827c9
출처 데이터셋
uspto-grants-1984_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04430339

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