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Potassium Carbonate → Methyl 3-(2-Acetoxyethoxy)-2-(4-methoxy-6-methyl-2-pyrimidinyloxy)-3,3-diphenylpropionate

HRID 397330
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HRID 397330 반응식
[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH:9]([OH:14])[C:10]([O:12][CH3:13])=[O:11])(=[O:3])[CH3:2].C([O-])([O-])=O.[K+].[K+].CS([C:37]1[N:42]=[C:41]([O:43][CH3:44])[CH:40]=[C:39]([CH3:45])[N:38]=1)(=O)=O>CN(C=O)C.O>[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH:9]([O:14][C:37]1[N:42]=[C:41]([O:43][CH3:44])[CH:40]=[C:39]([CH3:45])[N:38]=1)[C:10]([O:12][CH3:13])=[O:11])(=[O:3])[CH3:2]
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6

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HCID 11430Potassium CarbonateHCID 27723804-Methoxy-6-methyl-2-(methylsulfonyl)pyrimidineHCID 15379666Methyl 3-(2-Acetoxyethoxy)-2-hydroxy-3,3-diphenylpropionate

생성물 1

HCID 15379667Methyl 3-(2-Acetoxyethoxy)-2-(4-methoxy-6-methyl-2-pyrimidinyloxy)-3,3-diphenylpropionate수율 90%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

4 g (11.1 mmol) of methyl 3-(2-acetoxyethoxy)-2-hydroxy-3,3-di-phenylpropionate were dissolved in 20 ml of DMF under N2, 770 mg (5.6 mmol) of K2CO3 and 2.24 g (11.1 mmol) of 2-methanesulfonyl-4-methoxy-6-methylpyrimidine were added, and the mixture was stirred at 80° C. for 2 h. It was subsequently diluted with 20 ml of H2O and extracted twice with 30 ml of diethyl ether, the organic phase was dried over MgSO4 and concentrated, and the residue was purified by chromatography on silica gel with ethyl acetate/cyclohexane mixtures. 4.8 g (90%) of a colorless oil were obtained.

후처리

  1. extractionextracted twice with 30 ml of diethyl ether
  2. dry with materialthe organic phase was dried over MgSO4
  3. concentrationconcentrated
  4. customthe residue was purified by chromatography on silica gel with ethyl acetate/cyclohexane mixtures

출처 및 근거

ORD 기록
ord-03b1439572b6444597f8fdae9cae1202
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06610691B1

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