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

HRID 1386152노트

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HRID 1386152 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
0 °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 250C. 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. waitAfter 2 h
  2. additionthe reaction mixture is poured
  3. filtrationthe solid is collected by suction filtration
  4. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-54265f70a7604630bd4363f0095a8374
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265410B1

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