Potassium Carbonate → HCID 14330010, 화합물

HRID 2164947노트

반응식

HRID 2164947 반응식
[CH2:1]([O:3][C:4](=[O:20])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:15])[CH3:14])=[C:9]([OH:16])[C:8]=1[CH2:17][CH2:18][CH3:19])[CH3:2].[S:21]([O:25][CH2:26][CH2:27][O:28][CH2:29][CH2:30][O:31][CH2:32][CH2:33]OS(=O)(=O)C)(=[O:24])(=[O:23])[CH3:22].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.CN(C)C=O.C(OCC)(=O)C.C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4](=[O:20])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:15])[CH3:14])=[C:9]([O:16][CH2:33][CH2:32][O:31][CH2:30][CH2:29][O:28][CH2:27][CH2:26][O:25][S:21]([CH3:22])(=[O:23])=[O:24])[C:8]=1[CH2:17][CH2:18][CH3:19])[CH3:2]

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 11077635Triethylene Glycol DimethanesulfonateHCID 13389144Ethyl (4-acetyl-3-hydroxy-2-propylphenoxy)acetate

생성물 1

HCID 14330010HCID 14330010, 화합물수율 53%

시약·촉매·용매 3

HCID 180Acetone용매HCID 6228Dimethylformamide용매HCID 21584019Toluene ethylacetate용매

실험 절차

A mixture of 3.3 g (0.012 mole) of (4-acetyl-3-hydroxy-2-propylphenoxy)acetic acid ethyl ester, 18.0 g (0.059) of triethyleneglycol dimesylate and 3.3 g (0.024 mole) of anhydrous potassium carbonate in 100 ml of anhydrous acetone and 45 ml of anhydrous dimethylformamide was stirred at reflux for 26 hours. The reaction mixture was concentrated in vacuo to yield an oil which was dissolved in 60% ethyl acetate-toluene and passed through a column of 60 g of silica gel. The eluent was concentrated in vacuo and purified by HPLC using 35% ethyl acetate-toluene to give 3.06 g (53% yield) of [4-acetyl-3-[2-[2-[2-[(methylsulfonyl)oxy]ethoxy]ethoxy]ethoxy]-2-propylphenoxy]acetic acid ethyl ester as an oil.

후처리

  1. temperatureat reflux for 26 hours
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. customto yield an oil which
  4. concentrationThe eluent was concentrated in vacuo
  5. custompurified by HPLC

출처 및 근거

ORD 기록
ord-fdff84ae38dd499f8e54f45cad9106fc
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04507498

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