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Benzoyl Peroxide → HCID 22648121, 화합물

HRID 394093
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HRID 394093 반응식
[Cl:1][C:2]1[C:7]([CH3:8])=[C:6]([C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=2[F:16])[N:5]=[C:4]([S:17][CH3:18])[N:3]=1.[Br:19]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:19][CH2:8][C:7]1[C:2]([Cl:1])=[N:3][C:4]([S:17][CH3:18])=[N:5][C:6]=1[C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=1[F:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 22648011HCID 22648011, 화합물

생성물 1

HCID 22648121HCID 22648121, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

A suspension of 5.4 g of 4-chloro-6-(2,4-difluorophenyl)-5-methyl-2-(methylthio)pyrimidine. 3.69 g of N-bromosuccinimide, and 460 mg of benzoyl peroxide in 75 mL of CCl4 was heated to reflux and stirred at this temperature for 6 h, then cooled in the freezer for 1 h. The solids were filtered and washed liberally with cold CCl4, and the filtrate was concentrated. The residue was purified by flash chromatography on a Biotage 40M column, eluting with a gradient system of 99:1 to 97:3 hexanes-acetone to yield the title compound. Mass spectrum (ESI) 367 (M+1).

후처리

  1. temperatureto reflux
  2. temperaturecooled in the freezer for 1 h
  3. filtrationThe solids were filtered
  4. washwashed liberally with cold CCl4
  5. concentrationthe filtrate was concentrated
  6. customThe residue was purified by flash chromatography on a Biotage 40M column
  7. washeluting with a gradient system of 99:1 to 97:3 hexanes-acetone

출처 및 근거

ORD 기록
ord-31a0fabcabc74fc48652363a2afc6799
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06809199B2

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