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4-Bromostyrene → HCID 58288379、化合物

HRID 1475633
ノート
印刷プレビュー

反応式

HRID 1475633 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[CH2:7])=[CH:4][CH:3]=1.[FH:10].F.F.C(N(CC)CC)C.[Br:20]N1C(=O)CCC1=O>ClCCl>[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]([F:10])[CH2:7][Br:20])=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 162634-BromostyreneHCID 67184N-bromobutanimideHCID 175505N,N-Diethylethanamine trihydrofluoride

生成物 1

HCID 58288379HCID 58288379、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

5.0 g (27.31 mmol) of 4-bromostyrene were dissolved in 40 ml of dichloromethane, the mixture was cooled to 0° C. and 13.21 g (81.94 mmol) of triethylamine trihydrofluoride were added. 5.83 g (32.78 mmol) of N-bromosuccinimide were then added in three portions. The mixture was stirred at RT overnight. After dilution with dichloromethane, the reaction mixture was added to ice-water. The organic phase was washed successively with 1 N hydrochloric acid, water and saturated sodium bicarbonate solution, dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified by chromatography on silica gel (mobile phase pentane). This gave 4.14 g (53.8% of theory) of the title compound.

後処理

  1. washThe organic phase was washed successively with 1 N hydrochloric acid, water and saturated sodium bicarbonate solution
  2. dry with materialdried over magnesium sulphate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by chromatography on silica gel (mobile phase pentane)

出典と根拠

ORDレコード
ord-e5fca9cc6a434cff9bf2166feed5657d
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018258B2

反応ノート

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