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1,3-Dibromo-5,5-dimethylhydantoin → HCID 67175327, 화합물

HRID 1791886
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HRID 1791886 반응식
[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:5]=1[NH:11][C:12](=[O:15])[CH2:13][CH3:14].[Br:17]N1C(C)(C)C(=O)N(Br)C1=O>C(Cl)(Cl)Cl.C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:9]=[C:8]([CH2:10][Br:17])[CH:7]=[CH:6][C:5]=1[NH:11][C:12](=[O:15])[CH2:13][CH3:14]
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참가 물질

6

반응물 2

HCID 64791,3-Dibromo-5,5-dimethylhydantoinHCID 43623650HCID 43623650, 화합물

생성물 1

HCID 67175327HCID 67175327, 화합물수율 106.6%

시약·촉매·용매 3

HCID 7187Benzoyl Peroxide촉매HCID 5943Carbon Tetrachloride용매HCID 6212Chloroform용매

실험 절차

The radical bromination was performed as described by Patil et al. 1989: 5-Methyl-2-propionylamino-benzoic acid methyl ester (8.85 g, 40 mmol) and 1,3-dibromo-5,5-dimethyl hydantoin (DDH) (5,72 g, 20 mmol) in a mixture of CHCl3 (500 mL) and CCl4 (500 mL) was heated to reflux. Every 60 minutes 50 mg of dibenzoyl peroxide was added for six hours and then the reaction mixture was left at reflux over night. It was then allowed to reach room temperature and the solvents were removed by evaporation. Chromatography using silica gel 60 and heptane/ethyl acetate (18:2 ->17:3 ->16:4) as eluent afforded the pure title compound (6.40 g, 53%).

후처리

  1. temperaturewas heated to reflux
  2. waitthe reaction mixture was left
  3. temperatureat reflux over night
  4. customto reach room temperature
  5. customthe solvents were removed by evaporation

출처 및 근거

ORD 기록
ord-badfb920f6794f76916d9157a13ee71c
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074831B2

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