Water → 5-Amino-7,8-dihydro-8-(2-methoxyethyl)-7-oxo-2-phenylpyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

HRID 2058384노트

반응식

HRID 2058384 반응식
[C:1]([C:3]1[C:4]([NH:15][CH2:16][CH2:17][O:18][CH3:19])=[N:5][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:7][CH:8]=1)#[N:2].[CH2:20]([O:22]CC)[CH3:21].C([CH:27]([C:31](Cl)=[O:32])[C:28](Cl)=[O:29])C.O>C(O)C.C(O)(=O)C>[CH2:20]([O:22][C:31]([C:27]1[C:28](=[O:29])[N:15]([CH2:16][CH2:17][O:18][CH3:19])[C:4]2[N:5]=[C:6]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[N:7]=[CH:8][C:3]=2[C:1]=1[NH2:2])=[O:32])[CH3:21]

참가 물질

7

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 109209242-Ethylpropanedioyl dichlorideHCID 127840885-Cyano-4-(2-methoxyethylamino)-2-phenyl pyrimidine

생성물 1

HCID 127841045-Amino-7,8-dihydro-8-(2-methoxyethyl)-7-oxo-2-phenylpyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 702Ethanol용매

실험 절차

To 9.3 g. (0.037 mole) of 5-cyano-4-(2-methoxyethylamino)-2-phenyl pyrimidine in 350 ml. of diethyl ether was added 2.8 g. (0.019 mole) of ethyl malonyl chloride and this mixture was stirred at room temperature for 4.5 hours. Then the solid material was filtered off and the filtrate evaporated to dryness. Ethanol was added until a solution was obtained and this solution was added to 0.85 g. (0.057 mole) of Na in ethanol and stirred 20 minutes. A little water was added and the solution was acidified with acetic acid. The solid product was collected on a suction filter and recrystallized from ethanol to give 2.0 g. of product--m.p. 245°-247° C.

후처리

  1. filtrationThen the solid material was filtered off
  2. customthe filtrate evaporated to dryness
  3. additionEthanol was added until a solution
  4. customwas obtained
  5. additionthis solution was added to 0.85 g
  6. customThe solid product was collected on a suction
  7. filtrationfilter
  8. customrecrystallized from ethanol
  9. customto give 2.0 g

출처 및 근거

ORD 기록
ord-d367b2069d264931af97e50633e3c66f
출처 데이터셋
uspto-grants-1980_07
특허 번호
US04215216

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