Hydrochloric Acid → 1-Pyrimid-2-yl-4-phenyl-pyrazolin-5-one

HRID 977934

反応式

HRID 977934 の反応式
O[CH:2]=[C:3]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:4]([O:6]CC)=O.[NH:15]([C:17]1[N:22]=[CH:21][CH:20]=[CH:19][N:18]=1)[NH2:16].[OH-].[Na+].Cl>C(O)C.O>[N:18]1[CH:19]=[CH:20][CH:21]=[N:22][C:17]=1[N:15]1[C:4](=[O:6])[C:3]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)=[CH:2][NH:16]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 3465582-HydrazinylpyrimidineHCID 70430766Ethyl 3-hydroxy-2-phenylprop-2-enoate

生成物 1

HCID 135904631-Pyrimid-2-yl-4-phenyl-pyrazolin-5-one収率 63%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

19.2 g (0.1 mol) of ethyl α-hydroxymethylene-phenylacetate and 11 g (0.1 mol) of 2-hydrazino-pyrimidine in 150 ml of ethanol are boiled under reflux for 3 hours. The mixture is cooled to room temperature, and 9 g (0.1 mol) of concentrated sodium hydroxide solution are then added dropwise, while stirring. Stirring is then continued for 2 hours at room temperature, and the mixture is then boiled under reflux for 2 hours. The mixture is neutralized with concentrated hydrochloric acid, and diluted with 1 l of water. The precipitated crystals are filtered off under suction and dried in the air. 15 g (63% of theory) of 1-pyrimid-2-yl-4-phenyl-pyrazolin-5-one of melting point 159° to 160° C. (from ethanol) are obtained.

後処理

  1. temperatureunder reflux for 3 hours
  2. stirringStirring
  3. temperatureunder reflux for 2 hours
  4. filtrationThe precipitated crystals are filtered off under suction
  5. customdried in the air

出典と根拠

ORDレコード
ord-07fe76161f154dd9abfaa95f5a5917c3
出典データセット
uspto-grants-1987_05
特許番号
US04663327

関連ノート

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