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HCID 54296870, 화합물 → 1,4-Dihydro-2,6-dimethyl-3,5-dinitro-4-(3-nitrophenyl)pyridine

HRID 371415
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HRID 371415 반응식
[N+:1]([C:4]([C:15](=O)[CH3:16])=[CH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=1)([O-:3])=[O:2].[NH2:18][C:19]([CH3:24])=[CH:20][N+:21]([O-:23])=[O:22]>C(O)C>[CH3:16][C:15]1[NH:18][C:19]([CH3:24])=[C:20]([N+:21]([O-:23])=[O:22])[CH:5]([C:6]2[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=2)[C:4]=1[N+:1]([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 54296870HCID 54296870, 화합물HCID 714047121-Nitroprop-1-en-2-amine

생성물 1

HCID 131211851,4-Dihydro-2,6-dimethyl-3,5-dinitro-4-(3-nitrophenyl)pyridine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

23.6 g (0.1 mol) of 2-nitro-1-(3nitrophenyl)-but-1-ene-3-one and 10.2 g (0.1 mol) of 2-amino-1-nitro-prop-1-ene in 150 ml of ethanol were heated under reflux for 12 hours. After the mixture had cooled, the solvent was distilled off in vacuo, and the oily residue was taken up in chloroform, and was chromatographed on a silica gel column, using chloroform with the addition of methanol. The product formed yellow crystals of melting point 237°-240° C. (decomposition) in isopropanol.

후처리

  1. temperatureunder reflux for 12 hours
  2. temperatureAfter the mixture had cooled
  3. distillationthe solvent was distilled off in vacuo
  4. customwas chromatographed on a silica gel column
  5. additionwith the addition of methanol
  6. customThe product formed yellow crystals of melting point 237°-240° C. (decomposition) in isopropanol

출처 및 근거

ORD 기록
ord-e39d3ab89ae744699da76c9bfb4b04f5
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04532248

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