Water → (6-Nitro-7-fluoro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl ester

HRID 1289453노트

반응식

HRID 1289453 반응식
[CH2:1]([O:3][P:4]([CH2:9][N:10]1[C:19]2[C:14](=[CH:15][CH:16]=[C:17]([F:20])[CH:18]=2)[NH:13][C:12](=[O:21])[C:11]1=[O:22])(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].F[B-](F)(F)F.[O:28]=[N+:29]=[O:30].O>C(Cl)Cl>[CH2:6]([O:5][P:4]([CH2:9][N:10]1[C:19]2[C:14](=[CH:15][C:16]([N+:29]([O-:30])=[O:28])=[C:17]([F:20])[CH:18]=2)[NH:13][C:12](=[O:21])[C:11]1=[O:22])(=[O:8])[O:3][CH2:1][CH3:2])[CH3:7]

참가 물질

5

반응물 3

HCID 962WaterHCID 11073463Nitronium tetrafluoroborateHCID 15281076(7-Fluoro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)-methanephosphonic acid diethyl ester

생성물 1

HCID 17800809(6-Nitro-7-fluoro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl ester수율 50.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

615 mg of (7-fluoro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl ester is mixed in 60 ml of methylene chloride with 743 mg of nitronium tetrafluoroborate. The batch is stirred for 2 hours at room temperature. It is mixed with 50 ml of water and, after separation of the organic phase, it is extracted three times with methylene chloride. The collected organic phase is dried, filtered and concentrated by evaporation. The residue is chromatographed on silica gel with methylene chloride:ethanol=10:1. 350 mg of (6-nitro-7-fluoro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)-methanephosphonic acid diethyl ester is obtained.

후처리

  1. customafter separation of the organic phase, it
  2. extractionis extracted three times with methylene chloride
  3. customThe collected organic phase is dried
  4. filtrationfiltered
  5. concentrationconcentrated by evaporation
  6. customThe residue is chromatographed on silica gel with methylene chloride

출처 및 근거

ORD 기록
ord-a44b092851d6491cba7b4819531ae8b2
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750525

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