Methylamine → n2-Methyl-5-nitropyrimidine-2,4-diamine

HRID 453380노트

반응식

HRID 453380 반응식
Cl[C:2]1[N:7]=[C:6]([NH2:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.[CH3:12][NH2:13]>O>[CH3:12][NH:13][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1

참가 물질

4

반응물 2

HCID 6329Methylamine2회HCID 747162-Chloro-5-nitropyrimidin-4-amine

생성물 1

HCID 255555n2-Methyl-5-nitropyrimidine-2,4-diamine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 2-chloro-5-nitropyrimidin-4-amine (1.0 g, 5.8 mmol) and methylamine (2.0 M solution in THF, 14 mL, 28 mmol) was allowed to stir in a sealed vessel for 1 h. The mixture was then heated to 60 deg. C. for 30 min. The reaction was cooled to ambient temperature, and an additional amount of methylamine (2.0 M solution in THF, 8 mL, 16 mmol) was added and the reaction was sealed and heated to 60 deg. C. for 30 min. The reaction was cooled, diluted with water, and the precipitate was collected by filtration. The solid was rinsed with small portions of water followed by diethyl ether. The material was dried in under reduced pressure to give N2-methyl-5-nitropyrimidine-2,4-diamine 48 as a light yellow solid. MS (ES'): 170 (M+H)+; Calc. for C5H7N5O2=169.14.

후처리

  1. temperatureThe mixture was then heated to 60 deg. C
  2. waitfor 30 min
  3. customthe reaction was sealed
  4. temperatureheated to 60 deg. C
  5. waitfor 30 min
  6. temperatureThe reaction was cooled
  7. filtrationthe precipitate was collected by filtration
  8. washThe solid was rinsed with small portions of water
  9. customThe material was dried in under reduced pressure

출처 및 근거

ORD 기록
ord-d80c55dd783648f9b1fc67ac025781d0
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492404B2

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