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Potassium Carbonate → Benzyl 4-methoxycarbonylmethyloxyphenylacetate

HRID 1940524
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HRID 1940524 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:25][O:26][C:27](=[O:30])[CH2:28]Br>CN(C)C=O>[CH3:25][O:26][C:27]([CH2:28][O:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([O:11][CH2:12][C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)=[O:10])=[CH:6][CH:7]=1)=[O:30]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 11107524Benzyl 2-(4-hydroxyphenyl)acetate

생성물 1

HCID 53972878Benzyl 4-methoxycarbonylmethyloxyphenylacetate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 8.4 g (0.035 Mol) of benzyl 4-hydroxyphenylacetate and 4.8 g (0.035 Mol) of dried potassium carbonate in 100 ml of dimethylformamide are added slowly, after 45 minutes stirring at ambient temperature, 5.3 g (0.038 Mol) of methylbromoacetate and the mixture is then heated to 80° C. for 5 minutes whilst stirring continues. It is then stirred overnight at ambient temperature. The solid matter is filtered off and the mother liquor is evaporated to dryness under reduced pressure. The residue is purified over a silica gel column, using methylene chloride as eluant. Yield: 7.9 g amorphous solid (72.9% of theory).

후처리

  1. additionare added slowly, after 45 minutes
  2. stirringwhilst stirring
  3. stirringIt is then stirred overnight at ambient temperature
  4. filtrationThe solid matter is filtered off
  5. customthe mother liquor is evaporated to dryness under reduced pressure
  6. customThe residue is purified over a silica gel column

출처 및 근거

ORD 기록
ord-b89f86951dee4782b9c93b1d458a2297
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05700801

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