Diethyl Ether → Methyl 4-oxo-4-(4-phenoxyphenyl)but-2-enoate

HRID 2418150노트

반응식

HRID 2418150 반응식
[O:1]([C:8]1[CH:20]=[CH:19][C:11]([C:12]([CH:14]=[CH:15][C:16]([OH:18])=[O:17])=[O:13])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:21](=O)([O-])[O-].[Li+].[Li+].CI.C(OCC)C>CN(C)C=O>[O:1]([C:8]1[CH:20]=[CH:19][C:11]([C:12]([CH:14]=[CH:15][C:16]([O:18][CH3:21])=[O:17])=[O:13])=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6328Methyl iodideHCID 11125Lithium CarbonateHCID 54511907HCID 54511907, 화합물

생성물 1

HCID 53908224Methyl 4-oxo-4-(4-phenoxyphenyl)but-2-enoate수율 92.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5.36 g of 3-(4-phenoxybenzoyl)acrylic acid were dissolved in 30 ml of dimethylformamide, then 1.48 g of lithium carbonate and 5.68 g of methyl iodide were added. The mixture was stirred at room temperature for 3 hours and then allowed to stand overnight. Diethyl ether was added to the reaction mixture, which was then washed, in turn, with water, a saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over magnesium sulfate. The diethyl ether was removed by evaporation under reduced pressure, and the residue was recrystallized from a mixture of benzene and hexane to give 5.24 g of methyl 3-(4-phenoxybenzoyl)acrylate.

후처리

  1. waitto stand overnight
  2. washwas then washed, in turn, with water
  3. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over magnesium sulfate
  4. customThe diethyl ether was removed by evaporation under reduced pressure
  5. customthe residue was recrystallized from a mixture of benzene and hexane

출처 및 근거

ORD 기록
ord-6cd6d1e61ab5435283adc3cd4410dba4
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04472316

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