Methyl iodide → 7-Amino-4-methylthiopyrido[4,3-d]pyrimidine

HRID 50783

반응식

HRID 50783 반응식
[CH3:1]CN(CC)CC.[NH2:8][C:9]1[N:18]=[CH:17][C:16]2[C:15](=[S:19])[NH:14][CH:13]=[N:12][C:11]=2[CH:10]=1.CI>CS(C)=O>[NH2:8][C:9]1[N:18]=[CH:17][C:16]2[C:15]([S:19][CH3:1])=[N:14][CH:13]=[N:12][C:11]=2[CH:10]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 8471TriethylamineHCID 178507216HCID 178507216, 화합물

생성물 1

HCID 104425627-Amino-4-methylthiopyrido[4,3-d]pyrimidine수율 68.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
25 °C

실험 절차

NEt3 (6 mL, 43 mmol) is added to a solution of 7-amino-4-thiono-3H-pyrido[4,3-d]pyrimidine (0.77 g, 4.3 mmol) in DMSO (7 mL) stirred under N2 at 25° C. After the two phases have been stirred for 20 min, MeI (0.26 mL, 4.2 mmol) is added. After 2 h, the reaction mixture is poured onto stirring ice-water. Solid forms instantly. After further cooling at 0° C., the solid is collected by suction filtration and dried in a vacuum oven to give 7-amino-4-methylthiopyrido[4,3-d]pyrimidine (0.564 g, 68%). 1H NMR (DMSO) δ 8.98 (1H, s), 8.71 (1H, s), 6.94 (2H, brs), 6.49 (1H, s) 2.63 (3H, s).

후처리

  1. stirringAfter the two phases have been stirred for 20 min
  2. additionthe reaction mixture is poured
  3. temperatureAfter further cooling at 0° C.
  4. filtrationthe solid is collected by suction filtration
  5. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-3c1a5a338bbd43eca47ba4d10b6b6922
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713484B2

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