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Bromine → 2-(3',5'-Dichlorophenyl)-4,4-dimethyl-5-bromomethylenoxazoline hydrobromide

HRID 1780003
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HRID 1780003 반응식
[CH3:1][C:2]([NH:6][C:7](=[O:16])[C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[C:10]([Cl:15])[CH:9]=1)([CH3:5])[C:3]#[CH:4].[Br:17]Br>C(Cl)Cl.CCCCCC>[BrH:17].[Cl:14][C:12]1[CH:13]=[C:8]([C:7]2[O:16][C:3](=[CH:4][Br:17])[C:2]([CH3:1])([CH3:5])[N:6]=2)[CH:9]=[C:10]([Cl:15])[CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24408Bromine2회HCID 32154Propyzamide

생성물 1

HCID 677267812-(3',5'-Dichlorophenyl)-4,4-dimethyl-5-bromomethylenoxazoline hydrobromide수율 178.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8058Hexane용매

실험 절차

N- (1',1'-dimethylpropynyl)-3,5-dichlorobenzamide (40 gm, 0.156 m) was dissolved in methylene chloride (600 ml) and bromine (25 gm, 0.156 m) in methylene chloride (100 ml) was added gradually with stirring at room temperature. After the complete addition of the bromine, the mixture was stirred for another 15 minutes and diluted with hexane (500 ml). The yellowish-white precipitate which formed was filtered and dried to yield 58 gm of 2-(3',5'-dichlorophenyl)-4,4-dimethyl-5-bromomethylenoxazoline hydrobromide. The oxazoline hydrobromide (55 gm, 0.13 m) was added to concentrated sulfuric acid (200 ml) and stirred to obtain a clear solution. Water (20 ml) was added and the mixture heated at about 50° C. for about 24 hours. The mixture was then poured into ice water (about 2000 ml) and the white precipitate which formed was filtered and dried. Recrystallization from isopropanol, ether and hexane (1:1:2) yielded 21 gm of pure product.

후처리

  1. stirringthe mixture was stirred for another 15 minutes
  2. customThe yellowish-white precipitate which formed
  3. filtrationwas filtered
  4. customdried

출처 및 근거

ORD 기록
ord-d018dcc9ccaf4c66914144264432016f
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05629346

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