Potassium Carbonate → HCID 54137440, 화합물

HRID 327997노트

반응식

HRID 327997 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 54137440HCID 54137440, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9305be2b43fd44ff905d859107505550
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05273999

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