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Sodium Hydroxide → HCID 21223937, 화합물

HRID 2073207
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HRID 2073207 반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[N:16]2[C:17]3[N:12]([C:13]([C:18]4[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[CH:19]=4)=[CH:14][CH2:15]2)[N:11]=[CH:10][C:9]=3[C:8](=[O:28])[N:7]=1)=[O:4].[CH2:29]([N:36]1[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.[OH-].[Na+]>O1CCCC1>[O:28]=[C:8]1[N:7]=[C:6]([NH:5][C:3](=[O:4])[CH2:2][N:39]2[CH2:40][CH2:41][N:36]([CH2:29][C:30]3[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=3)[CH2:37][CH2:38]2)[N:16]2[C:17]3[N:12]([C:13]([C:18]4[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:26])([F:27])[F:25])[CH:19]=4)=[CH:14][CH2:15]2)[N:11]=[CH:10][C:9]1=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 759941-BenzylpiperazineHCID 15702796HCID 15702796, 화합물

생성물 1

HCID 21223937HCID 21223937, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A 1.000 g amount of 2-chloro-N-[3-oxo-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-5-yl]acetamide (prepared in the manner described in Example 31) was dissolved in 50 ml of dry tetrahydrofuran, then 430 mg of 1-benzylpiperazine was added to the mixture in one portion. The reaction mixture was heated at reflux for 16 hours. The mixture was cooled, made basic with 1N sodium hydroxide and extracted with chloroform. The solvent was evaporated and the solid was purified by conventional means to give 426 mg of the desired product as a brown solid.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 16 hours
  3. temperatureThe mixture was cooled
  4. extractionextracted with chloroform
  5. customThe solvent was evaporated
  6. customthe solid was purified by conventional means

출처 및 근거

ORD 기록
ord-ce6fd032742a494c95b2512740179226
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04916137

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