Hydrochloric Acid → HCID 22930700、化合物

HRID 1295273ノート

反応式

HRID 1295273 の反応式
[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([C:14]([O:16]CC2C=CC=CC=2)=[O:15])[N:11]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].O1CCCC1.Cl>C(O)C>[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([C:14]([OH:16])=[O:15])[N:11]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[N:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 22930777HCID 22930777、化合物

生成物 1

HCID 22930700HCID 22930700、化合物収率 95%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of benzyl 3-benzyloxy-1-phenyl-1H-pyrazole-5-carboxylate (50.88 g), 1N aqueous sodium hydroxide solution (200 ml), tetrahydrofuran (200 ml) and ethanol (200 ml) was refluxed at room temperature for 5 hrs. 1N Hydrochloric acid (200 ml) was added and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The obtained colorless crystals were collected by filtration to give 3-benzyloxy-1-phenyl-1H-pyrazole-5-carboxylic acid (36.91 g, yield 95%), which was then recrystallized from acetone-isopropyl ether. melting point: 163–164° C.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. filtrationThe obtained colorless crystals were collected by filtration

出典と根拠

ORDレコード
ord-1cc4649d58d140c699c53fbb2f56b95e
出典データセット
uspto-grants-2007_07
特許番号
US07241785B2

反応ノート

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