Potassium Carbonate → Methyl 2-(4-phenoxybut-1-yloxy)-phenylacetate

HRID 1085336

반응식

HRID 1085336 반응식
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([O:11][CH3:12])=[O:10].C(=O)([O-])[O-].[K+].[K+].[O:19]([CH2:26][CH2:27][CH2:28][CH2:29]Br)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C)C=O.C(OCC)C>[O:19]([CH2:26][CH2:27][CH2:28][CH2:29][O:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([O:11][CH3:12])=[O:10])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 70986(4-Bromobutoxy)benzeneHCID 89719Methyl (2-hydroxyphenyl)acetate

생성물 1

HCID 14550847Methyl 2-(4-phenoxybut-1-yloxy)-phenylacetate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

28.2 g (0.17 mole) of methyl 2-hydroxyphenylacetate, 25.8 g (0.19 mole) of potassium carbonate and 38.9 g (0.17 mole) of 4-phenoxybutyl bromide in 400 ml of dimethylformamide are stirred for 24 hours at 70° C. Thereafter, the solvent is stripped off and the residue is taken up in diethyl ether. The solution is extracted several times with water and saturated sodium carbonate solution and the organic phase is dried over MgSO4. The oil obtained after removal of the solvent is purified by chromatography over silica gel (cyclohexane/ethyl acetate). Yield: 31 g (58%).

후처리

  1. extractionThe solution is extracted several times with water and saturated sodium carbonate solution
  2. dry with materialthe organic phase is dried over MgSO4
  3. customThe oil obtained
  4. customafter removal of the solvent
  5. customis purified by chromatography over silica gel (cyclohexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-c21204cd35e44371820de599ad217de2
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05008438

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