Hydrochloric Acid → HCID 59469955, 화합물

HRID 1502196노트

반응식

HRID 1502196 반응식
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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86676047HCID 86676047, 화합물

생성물 1

HCID 59469955HCID 59469955, 화합물수율 69%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-86413646ef934f639cf9627e456002ef
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206202B2

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