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Potassium Hydroxide → 3,5-Di(carbazol-9-yl)benzoic acid

HRID 1037514
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반응식

HRID 1037514 반응식
[CH:1]1[C:13]2[N:12]([C:14]3[CH:15]=[C:16]([CH:21]=[C:22]([N:24]4[C:36]5[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=5[C:30]5[C:25]4=[CH:26][CH:27]=[CH:28][CH:29]=5)[CH:23]=3)[C:17]([O:19]C)=[O:18])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[OH-].[K+]>C1COCC1.CO.O>[CH:10]1[C:11]2[N:12]([C:14]3[CH:15]=[C:16]([CH:21]=[C:22]([N:24]4[C:25]5[CH:26]=[CH:27][CH:28]=[CH:29][C:30]=5[C:31]5[C:36]4=[CH:35][CH:34]=[CH:33][CH:32]=5)[CH:23]=3)[C:17]([OH:19])=[O:18])[C:13]3[C:5](=[CH:4][CH:3]=[CH:2][CH:1]=3)[C:6]=2[CH:7]=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 59638298Methyl 3,5-di(carbazol-9-yl)benzoate

생성물 1

HCID 596383053,5-Di(carbazol-9-yl)benzoic acid

시약·촉매·용매 2

HCID 962Water용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a solution of methyl 3,5-di(carbazol-9-yl)benzoate (1.0 g, 2.14 mmol) in THF/methanol (25.0 ml, 15:10) was added KOH (0.6 g, 10.69 mmol) in water (2.0 ml) at room temperature under stirring. The reaction was carried out at room temperature for 4.5 hours. The THF was evaporated. Next, methanol (20.0 ml) was added and then HCl water solution (80.0 ml; 15.0 ml of 36-38% HCl in 65.0 ml of water) was added. The mixture was stirred for 1 hour and a pale yellow solid product was obtained by filtration. The product was purified by recrystallization from acetone/water: 0.95 g (97.9%).

후처리

  1. customThe THF was evaporated
  2. additionNext, methanol (20.0 ml) was added
  3. additionHCl water solution (80.0 ml; 15.0 ml of 36-38% HCl in 65.0 ml of water) was added
  4. stirringThe mixture was stirred for 1 hour
  5. customa pale yellow solid product was obtained by filtration
  6. customThe product was purified by recrystallization from acetone/water

출처 및 근거

ORD 기록
ord-92b25e5c03a142ff9bc9b3b93c823ba6
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08546505B2

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