Potassium Nitrate → 7-Chloro-6,8-difluoro-5-nitro-1,4-dihydroquinoxaline-2,3-dione

HRID 1600709노트

반응식

HRID 1600709 반응식
[Cl:1][C:2]1[C:3]([F:15])=[C:4]2[C:9](=[CH:10][C:11]=1[F:12])[NH:8][C:7](=[O:13])[C:6](=[O:14])[NH:5]2.[N+:16]([O-])([O-:18])=[O:17].[K+]>OS(O)(=O)=O>[Cl:1][C:2]1[C:3]([F:15])=[C:4]2[C:9]([NH:8][C:7](=[O:13])[C:6](=[O:14])[NH:5]2)=[C:10]([N+:16]([O-:18])=[O:17])[C:11]=1[F:12]

참가 물질

4

반응물 2

HCID 24434Potassium Nitrate2회HCID 108235056-Chloro-5,7-difluoro-1,4-dihydroquinoxaline-2,3-dione

생성물 1

HCID 105166837-Chloro-6,8-difluoro-5-nitro-1,4-dihydroquinoxaline-2,3-dione수율 65%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a solution of 120 mg (5.16 mmol) of 6-chloro-5,7-difluoro-1,4-dihydroquinoxaline-2,3-dione in 1 mL of H2SO4 (97%) kept in an ice bath was added portionwise 60 mg (0.59 mmol) of KNO3. The solution was stirred at room temperature for 14 h and 60 mg of KNO3 was added. It was stirred at room temperature for 24 h, then diluted with ice-water (4 mL), filtered, washed with water, and dried to leave a yellow solid (94 mg, 65%). The solid was purified by NaOH/HCl precipitation to leave 63 mg of yellow solid; mp>250° C.; 1H NMR (DMSO-d6), 12.11 (mb, 1), 12.503 (s, 1).

후처리

  1. stirringIt was stirred at room temperature for 24 h
  2. filtrationfiltered
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-9db58aa0f1e9412295194c3ce55e385f
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05977107

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