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Potassium Carbonate → 1-Methyl-4-(4-nitrophenyl)-1,4-diazepane

HRID 1294398
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HRID 1294398 반응식
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].C(=O)([O-])[O-].[K+].[K+].[CH3:17][N:18]1[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>O>[CH3:17][N:18]1[CH2:24][CH2:23][CH2:22][N:21]([C:6]2[CH:5]=[CH:4][C:3]([N+:8]([O-:10])=[O:9])=[CH:2][CH:7]=2)[CH2:20][CH2:19]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 738951-Fluoro-2-nitrobenzeneHCID 2283491-Methylhomopiperazine

생성물 1

HCID 31247221-Methyl-4-(4-nitrophenyl)-1,4-diazepane수율 94.5%

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

Fluoronitrobenzene (10.3 g, 0.073 mol) is dissolved in water and then potassium carbonate (12.1 g, 0.0876 mol) is added. 1-Methyl[1,4]diazepane (10 g, 0.0876 mol) is introduced and then the reaction medium is heated under reflux (≅100° C.) for 5 hours. The medium is cooled. A precipitate forms, which is filtered and washed with water. A yellow solid is recovered, which is dried at 45° C. in a vacuum oven (16.21 g, yield=94.5%).

후처리

  1. temperaturethe reaction medium is heated
  2. temperatureThe medium is cooled
  3. filtrationA precipitate forms, which is filtered
  4. washwashed with water
  5. customA yellow solid is recovered
  6. customwhich is dried at 45° C. in a vacuum oven (16.21 g, yield=94.5%)

출처 및 근거

ORD 기록
ord-6fc27060344f44b5a5f009309b142a75
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07241317B2

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