Methylamine → 1-N'-[(6-chloropyridin-3-yl)methyl]-1-N-methyl-2-nitroethene-1,1-diamine

HRID 249508노트

반응식

HRID 249508 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][C:10](SC)=[CH:11][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1.[CH3:17][NH2:18]>CCO>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]([NH:18][CH3:17])=[CH:11][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 855929321-(6-Chloro-3-pyridylmethyl)amino-1-methylthio-2-nitroethylene

생성물 1

HCID 43256191-N'-[(6-chloropyridin-3-yl)methyl]-1-N-methyl-2-nitroethene-1,1-diamine수율 53.8%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

In 100 ml of EtOH was dissolved 1.2 g (4.6×10-3 mole) of 1-(6-chloro-3-pyridylmethyl)amino-1-methylthio-2-nitroethylene and on reflux, a solution of 0.84 g of 40% aqueous methylamine in 30 ml EtOH was added dropwise over 1 hour. After cooling, the reaction mixture was concentrated under reduced pressure to about 50 ml and the resulting crystals were collected by filtration and dried to give 0.6 g of the title compound as pale yellow needles.

후처리

  1. temperatureon reflux
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated under reduced pressure to about 50 ml
  4. filtrationthe resulting crystals were collected by filtration
  5. customdried

출처 및 근거

ORD 기록
ord-659fbe34b189419289ea8e87ff3e23ac
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05214152

반응 노트

불러오는 중…