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Sodium hydride → HCID 20356988, 화합물

HRID 2083573
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HRID 2083573 반응식
[CH2:1]1[O:13][C:12]2[CH:11]=[C:10]3[C:5]([C:6](=[O:17])[C:7]([C:14]([OH:16])=[O:15])=[CH:8][NH:9]3)=[CH:4][C:3]=2[O:2]1.[H-].[Na+].ClC(Cl)(Cl)S(O[CH2:26][C:27]([F:30])([F:29])[F:28])(=O)=O>CN(C)C=O>[CH2:1]1[O:13][C:12]2[CH:11]=[C:10]3[C:5]([C:6](=[O:17])[C:7]([C:14]([OH:16])=[O:15])=[CH:8][N:9]3[CH2:26][C:27]([F:30])([F:29])[F:28])=[CH:4][C:3]=2[O:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 900272,2,2-Trifluoroethyl trichloromethanesulphonateHCID 1522615,8-Dihydro-8-oxo-1,3-dioxolo(4,5-g)quinoline-7-carboxylic acid

생성물 1

HCID 20356988HCID 20356988, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 15.6 (0.06 mole) of 6,7-methylenedioxy-4(1H)-quinolone-3-carboxylic acid (J. Med. Chem. 11, 160 (1968)) and 1.5 g. (0.062 mole) of sodium hydride powder in 250 ml. of dimethyl formamide was heated with stirring for 0.5 hour at 80°-90° C. 2,2,2-Trifluoroethyl trichloromethanesulfonate (17.5 g. 0.62 mole) was then added dropwise. The temperature was maintained at 80°-90° for an additional two hours. The cooled mixture was poured into ice water and the solid product was isolated by filtration. It was recrystallized from ethanol. This product was identical to that obtained from Example 1.

후처리

  1. temperatureThe temperature was maintained at 80°-90° for an additional two hours
  2. customthe solid product was isolated by filtration
  3. customIt was recrystallized from ethanol
  4. customthat obtained from Example 1

출처 및 근거

ORD 기록
ord-847fb38641a1462c9dcd648e008e227e
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04086236

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