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

HRID 1059570ノート

反応式

HRID 1059570 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
25 °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 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).

後処理

  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

出典と根拠

ORDレコード
ord-4e5b38c176a74d5291dc22f77cbe1481
出典データセット
uspto-grants-2003_02
特許番号
US06521620B1

反応ノート

読み込み中…