Ethyl bromoacetate → Ethyl[(6,7-dichlorobenzo[b]thien-5-yl)oxy]acetate

HRID 370940

반응식

HRID 370940 반응식
[Cl:1][C:2]1[C:3]([OH:12])=[CH:4][C:5]2[CH:9]=[CH:8][S:7][C:6]=2[C:10]=1[Cl:11].Br[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:18]([O:17][C:15](=[O:16])[CH2:14][O:12][C:3]1[C:2]([Cl:1])=[C:10]([Cl:11])[C:6]2[S:7][CH:8]=[CH:9][C:5]=2[CH:4]=1)[CH3:19]

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 132899976,7-Dichloro-1-benzothiophene-5-ol

생성물 1

HCID 13289999Ethyl[(6,7-dichlorobenzo[b]thien-5-yl)oxy]acetate수율 63.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 3.6 g of 6,7-dichloro-5-hydroxybenzo[b]thiophene, 3.0 g of ethyl bromoacetate, 1.5 g of potassium carbonate and 40 ml of anhydrous dimethylformamide is stirred at 70°-80° for 16 hours. The cooled mixture is diluted with ice-water (200 g) and the solid collected by filtration. Recrystallization of the crude product from acetone-hexane gives 3.2 g of ethyl[(6,7-dichlorobenzo[b]thien-5-yl)oxy]acetate as yellowish needles, mp 92°-93°.

후처리

  1. filtrationthe solid collected by filtration
  2. customRecrystallization of the crude product from acetone-hexane

출처 및 근거

ORD 기록
ord-56941bab06ea4a2497e57e5f80a429b3
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528399

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