Water → HCID 58194202、化合物

HRID 68523ノート

反応式

HRID 68523 の反応式
[C:1]1([C:7]2[CH:20]=[CH:19][C:18]3[C:9](=[CH:10][C:11]4[C:16]([CH:17]=3)=[CH:15][C:14]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[CH:13][CH:12]=4)[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:27]N1C(=O)CCC1=O.O>CN(C)C=O>[Br:27][C:17]1[C:18]2[C:9]([CH:10]=[C:11]3[C:16]=1[CH:15]=[C:14]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH:13]=[CH:12]3)=[CH:8][C:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)=[CH:20][CH:19]=2

参加物

5

反応物 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 149154562,6-Diphenylanthracene

生成物 1

HCID 58194202HCID 58194202、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
60 °C

実験手順

First, 33.0 g of 2,6-diphenylanthracene were dissolved in 200 mL of N,N-dimethylformamide under heat, and then a solution of 18.0 g of N-bromosuccinimide in 20 mL of N,N-dimethylformamide was added to the solution. The mixture was stirred at 60° C. for 6 hours under heat. After having been cooled to room temperature, the reaction solution was poured into 1 L of water. The resultant solid was sequentially washed with methanol, water, and methanol. After that, the solid was repeatedly recrystallized with toluene and hexane and washed. Thus, 33.5 g of 9-bromo-2,6-diphenylanthracene were obtained (in 82% yield).

後処理

  1. temperatureunder heat
  2. temperatureunder heat
  3. temperatureAfter having been cooled to room temperature
  4. washThe resultant solid was sequentially washed with methanol, water, and methanol
  5. customAfter that, the solid was repeatedly recrystallized with toluene and hexane
  6. washwashed

出典と根拠

ORDレコード
ord-c256786fceaf4707a367cfde7c1799e0
出典データセット
uspto-grants-2014_09
特許番号
US08822041B2

反応ノート

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