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Dimethylformamide → 8-amino-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxamide

HRID 44600
ノート
印刷プレビュー

反応式

HRID 44600 の反応式
[NH2:1][C:2]1[N:11]=[CH:10][C:9]2[CH:8]=[CH:7][C:6]3[C:12]([C:16]([O:18]CC)=O)=[N:13][N:14]([CH3:15])[C:5]=3[C:4]=2[N:3]=1.C[N:22](C)C=O.[NH4+].[OH-]>CO>[NH2:1][C:2]1[N:11]=[CH:10][C:9]2[CH:8]=[CH:7][C:6]3[C:12]([C:16]([NH2:22])=[O:18])=[N:13][N:14]([CH3:15])[C:5]=3[C:4]=2[N:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 14923Ammonium HydroxideHCID 57444093Ethyl 8-amino-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate

生成物 1

HCID 574441008-amino-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxamide収率 50%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

2.5 g of ethyl 8-amino-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate (9.16 mmol) were dissolved in 40 mL of methanol, 40 mL of dimethylformamide and 50 mL of NH4OH 30% mixture. The mixture was maintained at 65° C. under stirring for a day. The solvent was then evaporated to dryness, the residue redissolved with dichloromethane and washed with water. The organic layer was dried over Na2SO4 and evaporated. The crude was triturated with diethyl ether and the product collected by filtration (50% yield).

後処理

  1. customThe solvent was then evaporated to dryness
  2. dissolutionthe residue redissolved with dichloromethane
  3. washwashed with water
  4. dry with materialThe organic layer was dried over Na2SO4
  5. customevaporated
  6. customThe crude was triturated with diethyl ether
  7. filtrationthe product collected by filtration (50% yield)

出典と根拠

ORDレコード
ord-fe63789c4a2047d6a979ae178973f972
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08541429B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート