Dimethylamine → 1-ethyl-N,N-dimethyl[1,2,4]triazolo[4,3-a]quinoxalin-4-amine

HRID 2412907ノート

反応式

HRID 2412907 の反応式
Cl[C:2]1[C:3]2[N:4]([C:12]([CH2:15][CH3:16])=[N:13][N:14]=2)[C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[CH3:17][NH:18][CH3:19]>CN(C)C=O>[CH3:17][N:18]([CH3:19])[C:2]1[C:3]2[N:4]([C:12]([CH2:15][CH3:16])=[N:13][N:14]=2)[C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2

参加物

4

反応物 2

HCID 674DimethylamineHCID 133857064-Chloro-1-ethyl-[1,2,4]triazolo[4,3-a]quinoxaline

生成物 1

HCID 8992951-ethyl-N,N-dimethyl[1,2,4]triazolo[4,3-a]quinoxalin-4-amine収率 42%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-Chloro-1-ethyl-[1,2,4]triazolo-[4,3-a]quinoxaline (1.2 g., 0.005 mole), the product of Example 4, and 676 mg. (0.015 mole) of anhydrous dimethylamine in N,N-dimethylformamide (50 ml.) were stirred at 0° C. for 30 minutes and at room temperature for 2 hours. The reaction mixture was poured over ice and stirred for 20 minutes. The precipitate which formed was separated by filtration, washed with water and air dried. Recrystallization from chloroform and then from chloroform/cyclohexane afforded 510 mg. (42% yield) of 4-dimethylamino-1-ethyl-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. 155°-8° C. Mass spectrum: m/e, 241 (P).

後処理

  1. additionThe reaction mixture was poured over ice
  2. customThe precipitate which formed
  3. customwas separated by filtration
  4. washwashed with water and air
  5. customdried
  6. customRecrystallization from chloroform
  7. customfrom chloroform/cyclohexane afforded 510 mg

出典と根拠

ORDレコード
ord-69cf0909fdf0440a9287fdc6214bf8c7
出典データセット
uspto-grants-1985_01
特許番号
US04495187

反応ノート

読み込み中…