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N-(2-chloro-5-pyridylmethyl)trimethylenediamine → 1-(2-Chloro-5-pyridylmethyl)-2-(nitroimino)tetrahydropyrimidine

HRID 359507
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HRID 359507 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][CH2:10][CH2:11][CH2:12][NH2:13])=[CH:4][N:3]=1.[N+:14]([NH:17][C:18](N)=N)([O-:16])=[O:15]>O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[CH2:10][CH2:11][CH2:12][NH:13][C:18]2=[N:17][N+:14]([O-:16])=[O:15])=[CH:4][N:3]=1
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참가 물질

4

반응물 2

HCID 10703172N-(2-chloro-5-pyridylmethyl)trimethylenediamineHCID 86287517Nitroguanidine

생성물 1

HCID 1363427891-(2-Chloro-5-pyridylmethyl)-2-(nitroimino)tetrahydropyrimidine수율 45.2%

시약·촉매·용매 1

HCID 962Water용매

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온도
80 °C

실험 절차

A solution composed of N-(2-chloro-5-pyridylmethyl)trimethylenediamine (10 g), nitroguanidine (5.7 g) and water (80 ml) was heated at 80° C. for 3 hours The reaction mixture was cooled to room temperature, and extracted twice with 50 ml of dichloromethane. Dichloromethane was distilled off from the extracts, and the tarry residue was purified by silica gel column chromatography to give almost colorless 1-(2-chloro-5-pyridylmethyl)-2-(nitroimino)tetrahydropyrimidine (6.1 g).

후처리

  1. temperaturewas cooled to room temperature
  2. extractionextracted twice with 50 ml of dichloromethane
  3. distillationDichloromethane was distilled off from the extracts
  4. customthe tarry residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-e60042c8a2864ecb9eb77f0402f10c37
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05001138

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