Water → HCID 58194202, 화합물

HRID 68516노트

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HRID 68516 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 58194202HCID 58194202, 화합물수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
60 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4daac58b54d84b05b9a00b1bfd35bf51
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822041B2

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