Methanol → 5,8-Dimethoxy-[1,2,4]triazolo[1,5-c]pyrimidin-2-amine

HRID 1099103노트

반응식

HRID 1099103 반응식
Cl[C:2]1[N:7]2[N:8]=[C:9]([NH2:11])[N:10]=[C:6]2[C:5]([O:12][CH3:13])=[CH:4][N:3]=1.[CH3:14][O-:15].[Na+].CO>C(#N)C>[CH3:14][O:15][C:2]1[N:7]2[N:8]=[C:9]([NH2:11])[N:10]=[C:6]2[C:5]([O:12][CH3:13])=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 569495765-Chloro-8-methoxy[1,2,4]triazolo[1,5-c]pyrimidin-2-amine

생성물 1

HCID 114468885,8-Dimethoxy-[1,2,4]triazolo[1,5-c]pyrimidin-2-amine수율 88%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

5-Chloro-8-methoxy[1,2,4]triazolo[1,5-c]pyrimidin-2-amine (4; 100 mg, 0.50 mmol) was suspended in acetonitrile (5 mL) at room temperature and treated with 25% sodium methoxide in methanol (200 mg, 2 eq). The resulting slurry was stirred at room temperature for 1.5 hours and then filtered. The solids were washed with water and dried to afford the title compound as a chalk-colored solid (87 mg, 88%) that was identical in HPLC retention to authentic 5,8-dimethoxy[1,2,4]triazolo[1,5-c]pyrimidin-2-amine (5): mp 185-186° C.; 1H NMR (DMSO-d6) δ 7.48 (s, 1H), 6.38 (br s, 2H), 4.04 (s, 3H), 3.88 (s, 3H); EIMS m/z 195.

후처리

  1. filtrationfiltered
  2. washThe solids were washed with water
  3. customdried

출처 및 근거

ORD 기록
ord-c3329b98ef704a1d8fb9eeb6e686e277
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143395B2

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