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

HRID 657681노트

반응식

HRID 657681 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a007f4c41d234b6b9c4f6c9e512cfbd7
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076344B2

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