Diethyl (ethoxymethylene)malonate → HCID 178469976, 화합물

HRID 386377

반응식

HRID 386377 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178469976HCID 178469976, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-cbc4fcad5bc1492d851e5efcf9e3c2eb
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372807B2

연결된 노트

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