Sodium Iodide → 6-Iodo-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidin-7-amine

HRID 657681ノート

反応式

HRID 657681 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([NH2:8])[N:5]2[N:9]=[CH:10][N:11]=[C:4]2[N:3]=1.[Na+].[I-:13].CC1C=CC(S([N-]Cl)(=O)=O)=CC=1.O.O.O.[Na+]>C(O)(=O)C>[I:13][C:7]1[C:2]([CH3:1])=[N:3][C:4]2[N:5]([N:9]=[CH:10][N:11]=2)[C:6]=1[NH2:8]

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 1695055-Methyl(1,2,4)triazolo(1,5-a)pyrimidin-7-amineHCID 517414chloramine-T trihydrate

生成物 1

HCID 667428896-Iodo-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidin-7-amine収率 88%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a stirring mixture of 3:05 g (20.4 mmol) of 5-methyl[1,2,4]triazolo[1,5-a]pyrimidin-7-amine (prepared as described in Kano; Makisumi; Chem. Pharm. Bull.; 6; 1958; 583, 585) in 50 mL of acetic acid at room temperature was added NaI (3.2 g, 21.5 mmol). Chloramine-T trihydrate (6.0 g, 21.5 mmol) was then added portion wise. The resulting mixture was then stirred for 1 h at room temperature. Most of the organic solvent was removed on a rotavap. The mixture was taken up in 40 mL of CH3CN and filtered. The solid collected was washed with diethyl ether and dried in vacuum oven to give the title compound as a light yellow solid (4.93 g, 88% yield).

後処理

  1. customMost of the organic solvent was removed on a rotavap
  2. filtrationfiltered
  3. customThe solid collected
  4. washwas washed with diethyl ether
  5. customdried in vacuum oven

出典と根拠

ORDレコード
ord-a007f4c41d234b6b9c4f6c9e512cfbd7
出典データセット
uspto-grants-2011_12
特許番号
US08076344B2

反応ノート

読み込み中…