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Toluene → HCID 22146252、化合物

HRID 1823701
ノート
印刷プレビュー

反応式

HRID 1823701 の反応式
[CH3:1][CH:2]([CH2:17][CH3:18])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[O:11][CH2:12][CH:13]([CH3:16])[CH2:14][CH3:15].C(#N)C.[Br:22]N1C(=O)CCC1=O.C1(C)C=CC=CC=1>O>[CH3:1][CH:2]([CH2:17][CH3:18])[CH2:3][O:4][C:5]1[CH:10]=[C:9]([Br:22])[CH:8]=[CH:7][C:6]=1[O:11][CH2:12][CH:13]([CH3:16])[CH2:14][CH3:15]
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

6

反応物 4

HCID 1140TolueneHCID 6342Acetonitrile2 回HCID 67184N-bromobutanimideHCID 22146239HCID 22146239、化合物

生成物 1

HCID 22146252HCID 22146252、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

1,2-Bis(2-methylbutyloxy)benzene (338 g, 1.35 mol) together with 2.5 l of acetonitrile was placed in a reaction vessel, cooled to 0° C. and admixed with 264 g (1.48 mol) of N-bromosuccinimide. The mixture was warmed to RT and stirred for another 90 minutes. After taking off the acetonitrile, the residue was admixed with toluene and water and the phases were separated. After shaking the aqueous phase with toluene and drying the organic phase over Na2SO4, the toluene was taken off. The crude product was purified by double fractional distillation under reduced pressure. This gave the product as a colorless oil (145° C., 1.3 mbar): 275 g (62%).

後処理

  1. temperatureThe mixture was warmed to RT
  2. customthe phases were separated
  3. stirringAfter shaking the aqueous phase with toluene
  4. dry with materialdrying the organic phase over Na2SO4
  5. distillationThe crude product was purified by double fractional distillation under reduced pressure

出典と根拠

ORDレコード
ord-4e6c824e384947cba43c6849e5aab398
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07041388B1

反応ノート

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