Dimethylformamide → HCID 13338435、化合物

HRID 2417688ノート

反応式

HRID 2417688 の反応式
Cl[C:2]1[C:3]2[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[C:4]=2[N:5]=[C:6]([CH3:8])[N:7]=1.[NH2:14][CH:15]([CH3:19])[C:16](=[O:18])[CH3:17].C(N([CH2:25][CH3:26])CC)C.CN(C)C=[O:30]>>[CH3:12][N:11]1[C:3]2[C:2]([NH:14][CH:15]([C:16]3([CH3:17])[O:30][CH2:25][CH2:26][O:18]3)[CH3:19])=[N:7][C:6]([CH3:8])=[N:5][C:4]=2[C:9]([CH3:13])=[N:10]1

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 44721173-Amino-2-butanoneHCID 133384077-Chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine

生成物 1

HCID 13338435HCID 13338435、化合物収率 87%

実験手順

A mixture of 9.5 g (0.05 mol) of 7-chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine (Example 3), 10 g (0.075 mol) of 3-amino-2-butanone, ethylene ketal, and 14 ml of triethylamine in 30 ml of dimethylformamide is stirred at 50°-55° C. for 24 hours. The mixture is evaporated in vacuo, the residue is dissolved in methylene dichloride and washed with ammonium hydroxide solution. The organic layer is dried over MgSO4 and evaporated in vacuo. The residue is crystallized from pet ether to give 12.6 g (87%) of 1,3,5-trimethyl-N-[1-(2-methyl-1,3-dioxolan-2-yl)ethyl]-1H-pyrazol[4,3-d]pyrimidin-7-amine, mp 101°-103° C.

後処理

  1. customThe mixture is evaporated in vacuo
  2. dissolutionthe residue is dissolved in methylene dichloride
  3. washwashed with ammonium hydroxide solution
  4. dry with materialThe organic layer is dried over MgSO4
  5. customevaporated in vacuo
  6. customThe residue is crystallized from pet ether

出典と根拠

ORDレコード
ord-9fa8df680800474a888a1a2228cdd425
出典データセット
uspto-grants-1984_09
特許番号
US04469868

反応ノート

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