Diethyl (ethoxymethylene)malonate → HCID 178469976、化合物

HRID 386377

反応式

HRID 386377 の反応式
Cl.[C:2]1([NH:12][NH2:13])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].C([O:22][CH:23]=[C:24]([C:30](OCC)=O)[C:25]([O:27][CH2:28][CH3:29])=[O:26])C>O>[OH:22][C:23]1[N:12]([C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH:5]=[CH:4][CH:3]=2)[N:13]=[CH:30][C:24]=1[C:25]([O:27][CH2:28][CH3:29])=[O:26]

参加物

5

反応物 3

HCID 6871Diethyl (ethoxymethylene)malonateHCID 11430Potassium CarbonateHCID 519949Hydrazine, 1-naphthalenyl-, hydrochloride (1:1)

生成物 1

HCID 178469976HCID 178469976、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of naphthalen-1-ylhydrazine hydrochloride (1 g, 5.1 mmol) and potassium carbonate (1.4 g, 10.3 mmol) in water (30 mL) was added diethyl ethoxymethylenemalonate (1.1 g, 5.1 mmol) at room temperature. The reaction mixture was stirred for 3 hours at room temperature and then extracted with ethyl acetate. The aqueous layer was acidified with 1N HCl to pH 2 and then extracted with ethyl acetate again. This organic layer was dried over sodium sulfate and concentrated to give ethyl 5-hydroxy-1-(naphthalen-1-yl)-1H-pyrazole-4-carboxylate as a solid.

後処理

  1. extractionextracted with ethyl acetate
  2. extractionextracted with ethyl acetate again
  3. dry with materialThis organic layer was dried over sodium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-cbc4fcad5bc1492d851e5efcf9e3c2eb
出典データセット
uspto-grants-2013_02
特許番号
US08372807B2

関連ノート

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