Dimethyl malonate → HCID 178424666、化合物

HRID 1970959ノート

反応式

HRID 1970959 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]([NH2:10])=[NH:9])[CH:5]=[CH:4][CH:3]=1.[C:11](OC)(=[O:17])[CH2:12][C:13](OC)=[O:14].C[O-].[Na+]>CO>[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[N:10]=[C:13]([OH:14])[CH:12]=[C:11]([OH:17])[N:9]=2)[CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 7943Dimethyl malonateHCID 10942334Sodium MethoxideHCID 142532006-Methylpicolinimidamide

生成物 1

HCID 178424666HCID 178424666、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of 6-methyl-pyridine-2-carboxamidine (step 2) (1.2 eq, 8.23 mmol, 1.41 g) in MeOH (5 ml) under an inert atmosphere of argon, at room temperature is treated with dimethyl malonate (1 eq, 6.86 mmol, 1.04 ml) and 0.5 M sodium methoxide in MeOH (3eq, 20.6 mmol, 41.2 ml). The resulting mixture is heated at reflux overnight and then allowed to cool to room temperature. The mixture is dry loaded onto silica and purification by flash chromatography eluting with 0-5% MeOH in DCM affords the title compound as a pale yellow solid [M+H]+=204.

後処理

  1. temperatureThe resulting mixture is heated
  2. temperatureat reflux overnight
  3. customThe mixture is dry loaded onto silica and purification by flash chromatography
  4. washeluting with 0-5% MeOH in DCM

出典と根拠

ORDレコード
ord-0342e93953a5425c988dd6c24183769b
出典データセット
uspto-grants-2013_04
特許番号
US08431578B2

反応ノート

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