Potassium Iodide → 2-Amino-3-(2-methylbenzylamino)pyrazine

HRID 4294

반응식

HRID 4294 반응식
[NH2:1][C:2]1[C:7](Cl)=[N:6][CH:5]=[CH:4][N:3]=1.[CH3:9][C:10]1[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=1[CH2:12][NH2:13].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O.O>[NH2:1][C:2]1[C:7]([NH:13][CH2:12][C:11]2[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=2[CH3:9])=[N:6][CH:5]=[CH:4][N:3]=1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 69932-MethylbenzylamineHCID 11430Potassium CarbonateHCID 2762242-Amino-3-chloropyrazine

생성물 1

HCID 201523282-Amino-3-(2-methylbenzylamino)pyrazine수율 19.7%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-amino-3-chloropyrazine (4.3 g), 2-methylbenzylamine (4.6 g), potassium carbonate (5.5 g), and potassium iodide (0.4 g) in N,N-dimethylformamide (43 ml) was refluxed for 24 hours under a nitrogen atmosphere and allowed to stand at room temperature. The mixture was poured into water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent to give 2-amino-3-(2-methylbenzylamino)pyrazine (1.4 g).

후처리

  1. temperaturewas refluxed for 24 hours under a nitrogen atmosphere
  2. customto stand at room temperature
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent

출처 및 근거

ORD 기록
ord-9d28aa19805e4a3182693ceb169ad3c2
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725601

연결된 노트

불러오는 중…