Hydrochloric Acid → HCID 59469955、化合物

HRID 1502196ノート

反応式

HRID 1502196 の反応式
C([N:4]1[C:16]2[CH:15]=[CH:14][C:13]([Si:17]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[C:8]([Si:36]([C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1)([C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[CH:9]=2)(=O)C.[OH-].[Na+].Cl>O1CCCC1>[C:30]1([Si:17]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:13]2[CH:14]=[CH:15][C:16]3[NH:4][C:5]4[C:10]([C:11]=3[CH:12]=2)=[CH:9][C:8]([Si:36]([C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)([C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)[C:49]2[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=2)=[CH:7][CH:6]=4)[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86676047HCID 86676047、化合物

生成物 1

HCID 59469955HCID 59469955、化合物収率 69%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The obtained 9-acetyl-3,6-bis(triphenylsilyl)carbazole (1.97 g) was dissolved in tetrahydrofuran (50 mL). A 50% by mass aqueous sodium hydroxide solution (1.1 g) was added to the solution. The resultant mixture was stirred at 50° C. for 3 hours and cooled to room temperature. Diluted hydrochloric acid was added thereto until the pH reached 5, followed by stirring for 30 min. The mixture was extracted with methylene chloride. The separated organic layer was washed with water and dried, and the methylene chloride was evaporated. The residue was purified with a recycle HPLC (name of apparatus: Recycling Preparative HPLC LC-9201, product of Japan Analytical Industry Co., Ltd., developing solvent: THF, flow rate: 3.5 mL/min), to thereby obtain 1.28 g of 3,6-bis(triphenylsilyl)carbazole as colorless powder.

後処理

  1. extractionThe mixture was extracted with methylene chloride
  2. washThe separated organic layer was washed with water
  3. customdried
  4. customthe methylene chloride was evaporated
  5. customThe residue was purified with a recycle HPLC (name of apparatus: Recycling Preparative HPLC LC-9201, product of Japan Analytical Industry Co., Ltd., developing solvent: THF, flow rate: 3.5 mL/min)

出典と根拠

ORDレコード
ord-86413646ef934f639cf9627e456002ef
出典データセット
uspto-grants-2015_12
特許番号
US09206202B2

反応ノート

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