Methyl Methanesulfonate → 4-Phenylamino-2-amino-1,6-dimethylpyrimidinium methanesulfonate

HRID 378955

반응식

HRID 378955 반응식
[C:1]1([NH:7][C:8]2[CH:13]=[C:12]([CH3:14])[N:11]=[C:10]([NH2:15])[N:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:16][S:17]([O:20]C)(=[O:19])=[O:18]>C(O)C>[CH3:16][S:17]([O-:20])(=[O:19])=[O:18].[C:1]1([NH:7][C:8]2[CH:13]=[C:12]([CH3:14])[N+:11]([CH3:16])=[C:10]([NH2:15])[N:9]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 4156Methyl Methanesulfonate2회HCID 6082032-Amino-4-phenylamino-6-methylpyrimidine

생성물 1

HCID 223940294-Phenylamino-2-amino-1,6-dimethylpyrimidinium methanesulfonate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Compound No. 46. A suspension of 4-phenylamino-2-amino-6-methylpyrimidine, Compound No. 45, (0.25 g) in ethanol (4 mL) was treated with methyl methanesulfonate (0.090 g) and heated at reflux for 5 days. Additional methyl methanesulfonate (0.090 g) was added and the mixture refluxed another 2 days. Concentration and recrystallization from a mixture of methanol, ethyl acetate, and tert-butyl ethyl ether gave 0.10 g of 4-phenylamino-2-amino-1,6-dimethylpyrimidinium methanesulfonate.

후처리

  1. temperatureheated
  2. temperatureat reflux for 5 days
  3. temperaturethe mixture refluxed another 2 days
  4. concentrationConcentration and recrystallization
  5. additionfrom a mixture of methanol, ethyl acetate, and tert-butyl ethyl ether

출처 및 근거

ORD 기록
ord-907ab1d159414431b2120ad2cb4c0668
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297253B1

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