Water → HCID 14012477, 화합물

HRID 568614노트

반응식

HRID 568614 반응식
Cl[C:2]1[C:16]([Cl:17])=[C:15]([OH:18])[CH:14]=[CH:13][C:3]=1[C:4](=[N:11][OH:12])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[H-].[Na+].Br[CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24].O>CN(C)C=O.C1(C)C=CC=CC=1>[CH2:26]([O:25][C:23](=[O:24])[CH2:22][O:18][C:15]1[CH:14]=[CH:13][C:3]2[C:4]([C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=3)=[N:11][O:12][C:2]=2[C:16]=1[Cl:17])[CH3:27]

참가 물질

7

반응물 4

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 24758Sodium hydride2회HCID 136393678HCID 136393678, 화합물

생성물 1

HCID 14012477HCID 14012477, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매2회

실험 절차

A solution of 2,3-dichloro-4-hydroxybenzophenone oxime and 2.6 g of sodium hydride in 50 ml of dimethylformamide and 50 ml of toluene is heated to 118° C. and maintained at this temperature for 50 minutes. Thereafter, the reaction is permitted to cool prior to the dropwise addition of 7.9 g of ethyl bromoacetate in 50 ml of dimethylformamide. After the addition is complete the reaction mixture is stirred at ambient temperature for 40 minutes. To the well stirred mixture water is added dropwise to decompose any excess sodium hydride. The toluene is evaporated under vacuum and the resulting precipitate is collected by filtration and then rinsed with ether to yield the product ethyl[(7-chloro-3-phenyl-1,2-benzisoxazol-6-yl)oxy]acetate having a melting point of 130° to 132° C.

후처리

  1. temperaturemaintained at this temperature for 50 minutes
  2. temperatureto cool
  3. additionAfter the addition
  4. additionis added dropwise
  5. customThe toluene is evaporated under vacuum
  6. filtrationthe resulting precipitate is collected by filtration
  7. washrinsed with ether

출처 및 근거

ORD 기록
ord-6fd268a9c34d45ee8782c940b997e608
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728662

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