Water → Ethyl-{[7-chloro-3-(2,3-dimethylphenyl)-1,2-benzisoxazol-6-yl]oxy}acetate

HRID 652872노트

반응식

HRID 652872 반응식
Cl[C:2]1[C:18]([Cl:19])=[C:17]([OH:20])[CH:16]=[CH:15][C:3]=1[C:4](=[N:13][OH:14])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:6]=1[CH3:12].[H-].[Na+].Br[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].O>CN(C=O)C>[CH2:28]([O:27][C:25](=[O:26])[CH2:24][O:20][C:17]1[CH:16]=[CH:15][C:3]2[C:4]([C:5]3[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:6]=3[CH3:12])=[N:13][O:14][C:2]=2[C:18]=1[Cl:19])[CH3:29]

참가 물질

6

반응물 4

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 24758Sodium hydrideHCID 136393680HCID 136393680, 화합물

생성물 1

HCID 14012495Ethyl-{[7-chloro-3-(2,3-dimethylphenyl)-1,2-benzisoxazol-6-yl]oxy}acetate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
130 °C

실험 절차

To a solution of 5 g of 2,3-dichloro-4-hydroxy-2',3'-dimethylbenzophenone oxime in 70 ml of DMF, 0.96 g of NaH is added. The internal temperature is held between 95°-120° C. for seven hours, then the mixture is heated at 130° C. for 1.5 hours. The reaction mixture is cooled and 2.94 g of ethyl bromoacetate is added dropwise. The mixture is stirred one hour and water is added dropwise. The product which forms is filtered off and recrystallized from 95% ethanol to yield ethyl-{[7-chloro-3-(2,3-dimethylphenyl)-1,2-benzisoxazol-6-yl]oxy}acetate, mp 89°-91° C.

후처리

  1. temperatureThe reaction mixture is cooled
  2. filtrationThe product which forms is filtered off
  3. customrecrystallized from 95% ethanol

출처 및 근거

ORD 기록
ord-74c4caef3e414ae283b3359dfa9b5d2c
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673746

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