홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Triethylamine → 2-Nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehyde

HRID 1649199
노트
인쇄 미리보기

반응식

HRID 1649199 반응식
[N+:1]([C:4]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[CH:8][C:5]=1[CH:6]=[O:7])([O-:3])=[O:2].C(N(CC)CC)C.[CH3:25][O:26][C:27]1[CH:28]=[C:29]([CH:33]=[CH:34][C:35]=1[O:36][CH3:37])[C:30](Cl)=[O:31]>CN(C=O)C>[N+:1]([C:4]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:13][CH2:14][N:15]([C:30](=[O:31])[C:29]3[CH:33]=[CH:34][C:35]([O:36][CH3:37])=[C:27]([O:26][CH3:25])[CH:28]=3)[CH2:16][CH2:17]2)=[CH:8][C:5]=1[CH:6]=[O:7])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 77070Veratroyl chlorideHCID 109893842-Nitro-5-piperazinylbenzaldehyde

생성물 1

HCID 132363012-Nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehyde수율 53%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

2-Nitro-5-piperazinylbenzaldehyde (5 g) was suspended in 50 ml of DMF and 6 ml of triethylamine was added to the suspension. A solution of 4.4 g of 3,4-dimethoxybenzoyl chloride in 20 ml of DMF was added dropwise thereto with ice cooling externally while stirring and the mixture was stirred at room temperature for 2 hours and poured into saturated saline and extracted with methylene chloride. After washing with water, the methylene chloride layer was dried over anhydrous sodium sulfate. Then, the solvent was removed by distillation and to the residue was added methyl alcohol and the mixture was heated and cooled and crystals which formed were recrystallized form DMF to give 4.5 g of 2-nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehyde, m.p. 196°-198° C., yellow crystal.

후처리

  1. stirringthe mixture was stirred at room temperature for 2 hours
  2. additionpoured into saturated saline
  3. extractionextracted with methylene chloride
  4. washAfter washing with water
  5. dry with materialthe methylene chloride layer was dried over anhydrous sodium sulfate
  6. customThen, the solvent was removed by distillation and to the residue
  7. additionwas added methyl alcohol
  8. temperaturethe mixture was heated
  9. temperaturecooled
  10. customcrystals which formed
  11. customwere recrystallized form DMF

출처 및 근거

ORD 기록
ord-4d3ce01e8b304e919e6c0f6711038b89
출처 데이터셋
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04415572

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트