Diethyl Malonate → HCID 2237931, 화합물

HRID 1156843노트

반응식

HRID 1156843 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].[CH3:17][C:18]1[CH:29]=[CH:28][C:21]([O:22][CH2:23][CH2:24][CH2:25][CH2:26]Br)=[CH:20][CH:19]=1>C(O)C>[CH2:1]([O:3][C:4](=[O:11])[CH:5]([CH2:26][CH2:25][CH2:24][CH2:23][O:22][C:21]1[CH:20]=[CH:19][C:18]([CH3:17])=[CH:29][CH:28]=1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2]

참가 물질

6

반응물 4

HCID 7761Diethyl MalonateHCID 137870Toluene, p-(4-bromobutoxy)-HCID 2723922Sodium ethoxideHCID 5360545Sodium

생성물 1

HCID 2237931HCID 2237931, 화합물수율 94.2%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

176.2 g of malonic acid diethyl ester are added dropwise at 50° C. to a sodium ethylate solution freshly prepared from 23 g of sodium and 500 ml of ethanol. The mixture is kept at this temperature for 2 hours, and 243.2 g of 4-(4-methylphenoxy)butyl bromide are then added dropwise. When the addition is complete, the obtained mixture is stirred at 60° C. for 3 hours, and substantially concentrated; 1 l of ice-water is then added and the mixture is extracted 3 times with a total of 1 liter of methylene chloride. The combined organic phases are dried over sodium sulfate, and the solvent and the excess malonic acid diethyl ester is distilled off in vacuo. 303.9 g of 4-(4-methylphenoxy)butylmalonic acid diethyl ester are obtained as pale yellow, oily residue.

후처리

  1. additionWhen the addition
  2. concentrationsubstantially concentrated
  3. addition1 l of ice-water is then added
  4. extractionthe mixture is extracted 3 times with a total of 1 liter of methylene chloride
  5. dry with materialThe combined organic phases are dried over sodium sulfate
  6. distillationthe solvent and the excess malonic acid diethyl ester is distilled off in vacuo

출처 및 근거

ORD 기록
ord-6e9d17dd544b4fcdb52f57daa4ccd1df
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04337267

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