methyl 3-benzyloxy-1-phenyl-1H-pyrazole-5-carboxylate → HCID 178498600、化合物

HRID 2221613ノート

反応式

HRID 2221613 の反応式
C([O:8][C:9]1[CH:13]=[C:12]([C:14]([O:16][CH3:17])=[O:15])[N:11]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:10]=1)C1C=CC=CC=1>[Pd].O1CCCC1>[OH:8][C:9]1[CH:13]=[C:12]([C:14]([O:16][CH3:17])=[O:15])[N:11]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:10]=1

参加物

4

反応物 1

HCID 22930789methyl 3-benzyloxy-1-phenyl-1H-pyrazole-5-carboxylate

生成物 1

HCID 178498600HCID 178498600、化合物収率 97%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of methyl 3-benzyloxy-1-phenyl-1H-pyrazole-5-carboxylate (15.00 g), 5% palladium on carbon (10.92 g) and tetrahydrofuran (200 mL) was stirred under a hydrogen atmosphere at room temperature for 1 hr. After removing palladium on carbon by filtration, the mother liquid was concentrated. The residue was subjected to silica gel column chromatography to give methyl 3-hydroxy-1-phenyl-1H-pyrazole-5-carboxylate (10.30 g, yield 97%) as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:2, v/v). The crystals were recrystallized from tetrahydrofuran-isopropyl ether. melting point: 227-228° C.

後処理

  1. customAfter removing palladium on carbon
  2. filtrationby filtration
  3. concentrationthe mother liquid was concentrated

出典と根拠

ORDレコード
ord-8790bbf7bccc4f668203a13e976a7ff4
出典データセット
uspto-grants-2008_05
特許番号
US07368578B2

反応ノート

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