Potassium Carbonate → HCID 14330011、化合物

HRID 2231475

反応式

HRID 2231475 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 14330011HCID 14330011、化合物収率 81.9%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6228Dimethylformamide溶媒

実験手順

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 40 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.

後処理

  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

出典と根拠

ORDレコード
ord-f3a8a76a61dc49fd88c483b4ba04cb61
出典データセット
uspto-grants-1988_11
特許番号
US04782176

関連ノート

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