Potassium Carbonate → HCID 54137440、化合物

HRID 1648049ノート

反応式

HRID 1648049 の反応式
[OH:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6](=[O:12])[O:7]2.Br[CH2:14][CH2:15][CH2:16][CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[CH2:21]([O:20][C:18](=[O:19])[CH2:17][CH2:16][CH2:15][CH2:14][O:1][C:2]1[C:3]2[CH:4]=[CH:5][C:6](=[O:12])[O:7][C:8]=2[CH:9]=[CH:10][CH:11]=1)[CH3:22]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 84580Ethyl 5-bromovalerateHCID 53181792H-1-Benzopyran-2-one, 5-hydroxy-

生成物 1

HCID 54137440HCID 54137440、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 2.25 g (18.6 mmol) of 5-hydroxycoumarin, 4.2 g (20 mmol) of ethyl 5-bromovalerate, 7.0 g (50 mmol) of anhydrous, granular potassium carbonate, and 10 mL of dimethyl sulfoxide was stirred at room temperature for 24 hr. The resulting slurry was filtered with suction and the solids washed well with ethyl acetate. The filtrate and washes were combined and poured into water and the mixture was worked-up with ethyl acetate in the usual manner. The semi-solid residue was triturated and washed with hexane giving 2.36 g (44%) of 5-[(2-oxo-2H-1-benzopyran-5-yl)oxy]pentanoic acid ethyl ester as a tan solid.

後処理

  1. filtrationThe resulting slurry was filtered with suction
  2. washthe solids washed well with ethyl acetate
  3. additionpoured into water
  4. customThe semi-solid residue was triturated
  5. washwashed with hexane giving 2.36 g (44%) of 5-[(2-oxo-2H-1-benzopyran-5-yl)oxy]pentanoic acid ethyl ester as a tan solid

出典と根拠

ORDレコード
ord-5398fe03126d4a11b4970729a5d64ac3
出典データセット
uspto-grants-1995_07
特許番号
US05434186

反応ノート

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