Benzoyl Peroxide → HCID 68632004、化合物

HRID 1809469ノート

反応式

HRID 1809469 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 68632004HCID 68632004、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ed7b6d142d744fc8a1e78924a64e69ba
出典データセット
uspto-grants-2013_01
特許番号
US08362030B2

反応ノート

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