Methanethiol → 1-(1-Methyl-4-pyrazolylmethyl)2-(nitromethylene)tetrahydropyrimidine

HRID 22210

반응식

HRID 22210 반응식
[CH3:1][N:2]1[CH:6]=[C:5]([CH2:7][NH:8][CH2:9][CH2:10][CH2:11][NH2:12])[CH:4]=[N:3]1.[N+:13]([CH:16]=[C:17](SC)SC)([O-:15])=[O:14].CS>C(O)C>[CH3:1][N:2]1[CH:6]=[C:5]([CH2:7][N:8]2[CH2:9][CH2:10][CH2:11][NH:12][C:17]2=[CH:16][N+:13]([O-:15])=[O:14])[CH:4]=[N:3]1

참가 물질

5

반응물 3

HCID 878MethanethiolHCID 836231,1-Bis(methylthio)-2-nitroethyleneHCID 14207161N-(1-methyl-4-pyrazolylmethyl)trimethylenediamine

생성물 1

HCID 702490871-(1-Methyl-4-pyrazolylmethyl)2-(nitromethylene)tetrahydropyrimidine수율 70.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 16.8 g of N-(1-methyl-4-pyrazolylmethyl)-trimethylenediamine, 16.5 g of 1-nitro-2,2-bis(methylthio)ethylene and 200 ml of ethanol was heated under reflux until the generation of methylmercaptan ceased. The mixture was cooled, and the precipitated crystals were collected by filtration. Washing with methanol gave 16.6 g of the desired 1-(1-methyl-4-pyrazolylmethyl)2-(nitromethylene)tetrahydropyrimidine as pale yellow crystals.

후처리

  1. temperaturewas heated
  2. temperatureThe mixture was cooled
  3. filtrationthe precipitated crystals were collected by filtration
  4. washWashing with methanol

출처 및 근거

ORD 기록
ord-2bc2df6bc147415a9b2cca3c9d532670
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05428032

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