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Diethyl (ethoxymethylene)malonate → HCID 15675226, 화합물

HRID 1090118
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HRID 1090118 반응식
C([O:8][C:9]1[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[CH:12][C:10]=1[NH2:11])C1C=CC=CC=1.C([O:20][CH:21]=[C:22]([C:28](OCC)=O)[C:23]([O:25][CH2:26][CH3:27])=[O:24])C>C1(OC2C=CC=CC=2)C=CC=CC=1>[CH2:26]([O:25][C:23]([C:22]1[C:21](=[O:20])[C:12]2[C:10](=[C:9]([OH:8])[C:15]([O:16][CH3:17])=[CH:14][CH:13]=2)[NH:11][CH:28]=1)=[O:24])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 13596187HCID 13596187, 화합물

생성물 1

HCID 15675226HCID 15675226, 화합물수율 42.7%

시약·촉매·용매 1

HCID 7583Diphenyl Ether용매

실험 절차

Two grams of 2-benzyloxy-3-methoxyaniline and 2.3 g of diethyl ethoxymethylenemalonate were heated at a temperature of 100°-120° C. for 1 hour. Fifty milliliter of diphenyl ether was added to the mixture, and the resulting mixture was further heated at 250°-270° C. for 1.5 hours. After the mixture was cooled down to room temperature, it was purified by silica gel column chromatography (Wako Gel C-200, 100 g). Elution with a mixed solvent of chloroform (95 parts) and methanol (5 parts) gave 980 mg of 3-ethoxycarbonyl-8-hydroxy-7-methoxy-4(1H)-quinolone.

후처리

  1. temperaturethe resulting mixture was further heated at 250°-270° C. for 1.5 hours
  2. customit was purified by silica gel column chromatography (Wako Gel C-200, 100 g)
  3. washElution with a mixed solvent of chloroform (95 parts) and methanol (5 parts)

출처 및 근거

ORD 기록
ord-ef8294e4d00340069049079b77a40ccc
출처 데이터셋
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05081121

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