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

HRID 127390
ノート
印刷プレビュー

反応式

HRID 127390 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9e151dde6d43438eb364f8630d58165a
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04255568

反応ノート

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