Water → benzofuran-2,3-dione 2-[O-(2-bromoethyl)-oxime] 3-(O-methyloxime)

HRID 2186678노트

반응식

HRID 2186678 반응식
[CH3:1][O:2][N:3]=[C:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]1=[N:13][OH:14].C(=O)([O-])[O-].[Na+].[Na+].[Br:21][CH2:22][CH2:23]Br.O>CN(C)C=O>[CH3:1][O:2][N:3]=[C:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]1=[N:13][O:14][CH2:23][CH2:22][Br:21]

참가 물질

6

반응물 4

HCID 962WaterHCID 78391,2-DibromoethaneHCID 10340Sodium CarbonateHCID 178502623HCID 178502623, 화합물

생성물 1

HCID 73782576benzofuran-2,3-dione 2-[O-(2-bromoethyl)-oxime] 3-(O-methyloxime)수율 70.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1 g (0.0052 mol) of benzofuran-2,3-dione 3-(O-methyloxime) 2-oxime with 1.5 g (0.0141 mol) of sodium carbonate and 3 g (0.016 mol) of 1,2-dibromoethane in 5 ml of dimethylformamide are stirred at 80° C. for 6 hours. The reaction mixture is subsequently poured into water and extracted with diethyl ether. The organic phase is washed with aqueous potassium hydroxide solution and dried over sodium sulphate. The solvent is distilled off under reduced pressure, giving 1.1 g (70.7% of theory) of crude benzofuran-2,3-dione 2-[O-(2-bromoethyl)-oxime] 3-(O-methyloxime) as a mixture of stereoisomers which is reacted further without any purification.

후처리

  1. extractionextracted with diethyl ether
  2. washThe organic phase is washed with aqueous potassium hydroxide solution
  3. dry with materialdried over sodium sulphate
  4. distillationThe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-7e4d97a86622499793133cbffb79603d
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06407097B1

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