8-Quinolinamine, 7-methyl- → 5-(8-Amino-7-methyl-5-quinolylmethyl)-2,4(1H,3H)-pyrimidinedione

HRID 34446

反応式

HRID 34446 の反応式
Cl.CN([CH2:5][C:6]1[C:7](=[O:13])[NH:8][C:9](=[O:12])[NH:10][CH:11]=1)C.[NH2:14][C:15]1[C:16]([CH3:25])=[CH:17][CH:18]=[C:19]2[C:24]=1[N:23]=[CH:22][CH:21]=[CH:20]2>C(O)CO>[NH2:14][C:15]1[C:16]([CH3:25])=[CH:17][C:18]([CH2:5][C:6]2[C:7](=[O:13])[NH:8][C:9](=[O:12])[NH:10][CH:11]=2)=[C:19]2[C:24]=1[N:23]=[CH:22][CH:21]=[CH:20]2

参加物

4

反応物 2

HCID 2315568-Quinolinamine, 7-methyl-HCID 122674355-[(dimethylamino)methyl]-1H-pyrimidine-2,4-dione;hydrochloride

生成物 1

HCID 201298195-(8-Amino-7-methyl-5-quinolylmethyl)-2,4(1H,3H)-pyrimidinedione収率 78%

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

A mixture of 8.36 g (0.0406 mole) of 5-[(dimethylamino)methyl]uracil hydrochloride (B. Roth, J. Z. Strelitz, and B. S. Rauckman, J. Med. Chem. 23, 379 (1980) and 6.43 g (0.0406 mole) of 8-amino-7-methylquinoline (R. Long and K. Schofield, J. Chem. Soc. 1953, 2350) in 60 ml of ethylene glycol under nitrogen was heated at 135° for 4 hours. The mixture was cooled and the precipitated solid was collected, washed with ethanol and ether and dried. This crude product was purified by suspension in 550 ml of boiling ethanol and collection of the insoluble product. Yield, 8.90 g of the title compound (78%) m.p. 302°-305° (dec.). Anal. Calcd for C21H20N4 : C, 76.89; H, 6.14; N, 17.06. Found: C, 76.82; H, 6.17; N, 17.04.

後処理

  1. temperatureThe mixture was cooled
  2. customthe precipitated solid was collected
  3. washwashed with ethanol and ether
  4. customdried
  5. customThis crude product was purified by suspension in 550 ml of boiling ethanol
  6. customcollection of the insoluble product
  7. customYield

出典と根拠

ORDレコード
ord-511a7405e34546f59e9f01059d84fb40
出典データセット
uspto-grants-1988_08
特許番号
US04761475

関連ノート

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