Malonamide → HCID 178513675, 화합물

HRID 1020806노트

반응식

HRID 1020806 반응식
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]

참가 물질

5

반응물 3

HCID 7911MalonamideHCID 701221,3-DimethyluracilHCID 2723922Sodium ethoxide

생성물 1

HCID 178513675HCID 178513675, 화합물수율 65%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9591e8f4d4994c639c588edce3d4aefc
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716478B2

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