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

HRID 1079424
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인쇄 미리보기

반응식

HRID 1079424 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

반응 조건

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. temperatureThe reaction mixture was 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-8b06d0a349494c3baa22420aa926b699
출처 데이터셋
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05580889

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