Malonamide → HCID 178513675、化合物

HRID 1020806ノート

反応式

HRID 1020806 の反応式
CN1[CH:7]=[CH:6][C:5](=[O:8])N(C)C1=O.[C:11]([NH2:17])(=[O:16])[CH2:12][C:13]([NH2:15])=[O:14].[O-]CC.[Na+]>CCO>[OH:14][C:13]1[N:15]=[C:5]([OH:8])[CH:6]=[CH:7][C:12]=1[C:11]([NH2:17])=[O:16]

参加物

5

反応物 3

HCID 7911MalonamideHCID 701221,3-DimethyluracilHCID 2723922Sodium ethoxide

生成物 1

HCID 178513675HCID 178513675、化合物収率 65%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of compound 1,3-dimethylpyrimidine-2,4(1H,3H)-dione (14 g, 0.1 mol), malonamide (45 g, 0.44 mol) and sodium ethoxide (34 g, 0.4 mol) in EtOH (500 mL) was refluxed for 20 mins. The mixture was cooled to r.t, quenched by water and acidified with 1 M HCl to pH=1-2. The solid was filtered and the filter cake was concentrated in vacuo to afford compound 2,6-dihydroxynicotinamide. (10 g, yield: 65%). 1H-NMR (400 MHz, DMSO-d6) δ (ppm) 7.90-7.88 (d, 1H), 5.66-5.64 (d, 1H).

後処理

  1. temperaturewas refluxed for 20 mins
  2. temperatureThe mixture was cooled
  3. customquenched by water
  4. filtrationThe solid was filtered
  5. concentrationthe filter cake was concentrated in vacuo

出典と根拠

ORDレコード
ord-9591e8f4d4994c639c588edce3d4aefc
出典データセット
uspto-grants-2014_05
特許番号
US08716478B2

反応ノート

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