Potassium Hydroxide → HCID 19805429、化合物

HRID 1681689ノート

反応式

HRID 1681689 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8]Br)=[CH:6][CH:5]=1)([O-:3])=[O:2].[C:12]([N:17]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:19](=[O:26])[NH:18]1)([O:14][CH2:15][CH3:16])=[O:13].[OH-].[K+]>C(O)C>[C:12]([N:17]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:19](=[O:26])[N:18]1[CH2:8][C:7]1[CH:10]=[CH:11][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)([O:14][CH2:15][CH3:16])=[O:13]

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 660114-Nitrobenzyl bromideHCID 584113Ethyl 3-oxo-2,3-dihydro-1H-indazole-1-carboxylate

生成物 1

HCID 19805429HCID 19805429、化合物収率 59%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4-Nitrobenzyl bromide (540 mg) was added to a mixture of 1,2-dihydro-1-carboethoxy-3H-indazol-3-one (206 mg) and potassium hydroxide (67 mg) in ethanol (10 ml). The mixture was heated under reflux for 30 minutes. The cooled solution was clarified by filtration and the filtrate was evaporated. The residue was purified by column chromatography using methylene chloride as eluant to give 1,2-dihydro-1-carboethoxy-2-(4-nitrobenzyl)-3H-indazol-3-one (Ex. 39) as a solid, m.p. 123-124° C. in 59% yield.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. filtrationThe cooled solution was clarified by filtration
  4. customthe filtrate was evaporated
  5. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-b5a0debec6f14606927ce7535fbf838d
出典データセット
uspto-grants-1992_12
特許番号
US05173496

反応ノート

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