Benzoyl Peroxide → HCID 68632004, 화합물

HRID 1809469노트

반응식

HRID 1809469 반응식
[Br:1][C:2]1[C:3]([CH3:13])=[C:4]([CH:9]=[C:10]([F:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].C1C(=O)N([Br:21])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[C:3]([CH2:13][Br:21])=[C:4]([CH:9]=[C:10]([F:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6]

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 68633230methyl 3-bromo-5-fluoro-2-methylbenzoate

생성물 1

HCID 68632004HCID 68632004, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

반응 조건

온도
0 °C

실험 절차

A suspension of (E4), NBS (1.2 eq.) and benzoyl peroxide (0.1 eq.) in CCl4 (0.28 M) was heated to reflux for 4.5 h. Afterwards, the reaction mixture was cooled down to 0° C. and the solid filtered off. The solid was washed with Et2O and the filtrate was washed sequentially with 1 M Na2S2O3, brine and dried (Na2SO4). Evaporation of the solvent under reduced pressure afforded the title compound that was used without further purification in the next step. 1H NMR (400 MHz, CDCl3, 300 K) δ 7.63 (1H, dd, J=8.6 and 2.8 Hz), 7.52 (1H, dd, J=7.4 and 2.8 Hz), 5.10 (2H, s), 3.97 (3H, s).

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 4.5 h
  3. filtrationthe solid filtered off
  4. washThe solid was washed with Et2O
  5. washthe filtrate was washed sequentially with 1 M Na2S2O3, brine
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-ed7b6d142d744fc8a1e78924a64e69ba
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362030B2

반응 노트

불러오는 중…