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

HRID 1037514
ノート
印刷プレビュー

反応式

HRID 1037514 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-92b25e5c03a142ff9bc9b3b93c823ba6
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546505B2

反応ノート

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