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

HRID 1386152ノート

反応式

HRID 1386152 の反応式
[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

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 8471TriethylamineHCID 178507216HCID 178507216、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
0 °C

実験手順

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)

後処理

  1. waitAfter 2 h
  2. additionthe reaction mixture is poured
  3. filtrationthe solid is collected by suction filtration
  4. customdried in a vacuum oven

出典と根拠

ORDレコード
ord-54265f70a7604630bd4363f0095a8374
出典データセット
uspto-grants-2001_07
特許番号
US06265410B1

反応ノート

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