Potassium Carbonate → HCID 14330011, 화합물

HRID 2164950

반응식

HRID 2164950 반응식
[CH3:1][O:2][C:3](=[O:23])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16](=[O:18])[CH3:17])=[C:12]([OH:19])[C:11]=1[CH2:20][CH2:21][CH3:22].[S:24]([O:28][CH2:29][CH2:30][O:31][CH2:32][CH2:33]OS(=O)(=O)C)(=[O:27])(=[O:26])[CH3:25].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.CN(C)C=O>[CH3:1][O:2][C:3](=[O:23])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16](=[O:18])[CH3:17])=[C:12]([O:19][CH2:33][CH2:32][O:31][CH2:30][CH2:29][O:28][S:24]([CH3:25])(=[O:27])=[O:26])[C:11]=1[CH2:20][CH2:21][CH3:22]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 147571Diethylene Glycol DimethanesulfonateHCID 14330007Methyl 6-(4-acetyl-3-hydroxy-2-propylphenoxy)hexanoate

생성물 1

HCID 14330011HCID 14330011, 화합물수율 81.9%

시약·촉매·용매 2

HCID 180Acetone용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4.0 g (0.012 mole) of 6-(4-acetyl-3-hydroxy-2-propylphenoxy)hexanoic acid methyl ester, 16.3 g (0.062 mole) of diethyleneglycol dimesylate and 3.4 g (0.024 mole) of anhydrous potassium carbonate in 90 ml of anhydrous acetone and 4 ml of anhydrous dimethylformamide was stirred at reflux for 22 hours. The solvents were removed in vacuo and the residue was treated with 100 ml of 50% ethyl acetate-hexane. Some of the residual starting dimesylate was insoluble and was removed by filtration. The filtrate was concentrated in vacuo and the residual oil was purified by HPLC to give 4.8 g (80% yield) of 6-[4-acetyl-3-[2-[2-[(methylsulfonyl)oxy]ethoxy]ethoxy]-2-propylphenoxy]hexanoic acid methyl ester as an oil.

후처리

  1. temperatureat reflux for 22 hours
  2. customThe solvents were removed in vacuo
  3. additionthe residue was treated with 100 ml of 50% ethyl acetate-hexane
  4. customwas removed by filtration
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residual oil was purified by HPLC

출처 및 근거

ORD 기록
ord-d5ae3efa277b499f9d06dc135a3872c3
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04507498

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