Diethyl Malonate → 4-((4,6-Dihydroxypyrimidin-2-yl)amino)benzonitrile

HRID 1908949ノート

反応式

HRID 1908949 の反応式
[C:1]([O:9]CC)(=O)[CH2:2][C:3]([O:5]CC)=O.[C:12]([C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:21]([NH2:23])=[NH:22])=[CH:16][CH:15]=1)#[N:13].[Na]>C(O)C>[OH:9][C:1]1[CH:2]=[C:3]([OH:5])[N:23]=[C:21]([NH:20][C:17]2[CH:18]=[CH:19][C:14]([C:12]#[N:13])=[CH:15][CH:16]=2)[N:22]=1

参加物

5

反応物 3

HCID 7761Diethyl MalonateHCID 5360545SodiumHCID 178510065HCID 178510065、化合物

生成物 1

HCID 1785100404-((4,6-Dihydroxypyrimidin-2-yl)amino)benzonitrile収率 93.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Diethyl malonate (30 gm) was added to 1-(4-cyanophenyl)guanidine (30 gm) at room temperature. A solution of sodium (17.2 gm) in ethanol (450 ml) was added to the above reaction mass. The contents were heated to reflux and maintained for 12 hours. Distilled off the solvent completely under vacuum and then added water (500 ml). The reaction mass was stirred for 30 minutes and filtered. The solid obtained was dried to obtain 40 gm of 4-(4,6-dihydroxypyrimidine-2-yl-amino)benzonitrile.

後処理

  1. temperatureThe contents were heated
  2. temperatureto reflux
  3. temperaturemaintained for 12 hours
  4. distillationDistilled off the solvent completely under vacuum
  5. filtrationfiltered
  6. customThe solid obtained
  7. customwas dried

出典と根拠

ORDレコード
ord-db95016f3c0e4cf9bc49e189d4ebbc5c
出典データセット
uspto-grants-2013_12
特許番号
US08598341B2

反応ノート

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