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Ethyl bromoacetate → HCID 14303535, 화합물

HRID 1723175
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HRID 1723175 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8](=[O:10])[CH:7]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:6]=2[CH:17]=1.[H-].[Na+].Br[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23]>CN(C)C=O>[CH2:25]([O:24][C:22](=[O:23])[CH2:21][C:7]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:6]2[CH:17]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][C:8]1=[O:10])[CH3:26]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 24758Sodium hydrideHCID 28767462(3H)-Benzofuranone, 5-chloro-3-phenyl-

생성물 1

HCID 14303535HCID 14303535, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
20 °C

실험 절차

A solution of 42.8 mmol of 5-chloro-2,3-dihydro-2-oxo-3-phenylbenzofuran in 50 ml of anhydrous dimethylformamide is added at room temperature to a suspension of 42.8 mmol of sodium hydride in 20 ml of anhydrous dimethylformamide. The mixture is stirred for one hour at 20° C. and 42.8 mmol of ethyl bromoacetate are added. The mixture is stirred for 12 hours at 20° C., the medium concentrated under vacuum, the residue taken up in 200 ml of 1% strength hydrochloric acid solution, the aqueous phase extracted with benzene, the organic phase dried over anhydrous sodium sulfate, the solvent evaporated off and the crystalline residue washed with a solution of ethyl ether and acetone (90:10). After filtration, 25.8 mmol of crystals are collected.

후처리

  1. stirringThe mixture is stirred for 12 hours at 20° C.
  2. concentrationthe medium concentrated under vacuum
  3. extractionthe aqueous phase extracted with benzene
  4. dry with materialthe organic phase dried over anhydrous sodium sulfate
  5. customthe solvent evaporated off
  6. washthe crystalline residue washed with a solution of ethyl ether and acetone (90:10)
  7. customare collected

출처 및 근거

ORD 기록
ord-b492761ff00c4b2c8b476e1201508d11
출처 데이터셋
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04859700

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