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Hydrochloric Acid → 7-Fluoro-6-hydroxy-5-nitro-1,4-dihydroquinoxaline-2,3-dione

HRID 1600735
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인쇄 미리보기

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HRID 1600735 반응식
F[C:2]1[C:3]([N+:15]([O-:17])=[O:16])=[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.[OH-:18].[Na+].Cl>O>[F:12][C:11]1[CH:10]=[C:9]2[C:4]([NH:5][C:6](=[O:14])[C:7](=[O:13])[NH:8]2)=[C:3]([N+:15]([O-:17])=[O:16])[C:2]=1[OH:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 108002536,7-Difluoro-5-nitro-1,4-dihydro-2,3-quinoxalinedione

생성물 1

HCID 211899797-Fluoro-6-hydroxy-5-nitro-1,4-dihydroquinoxaline-2,3-dione수율 80.4%

시약·촉매·용매 1

HCID 962Water용매

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온도
105 °C

실험 절차

A mixture of 24 mg (0.098 mmol) of 6,7-difluoro-5-nitro-1,4-dihydroquinoxaline-2,3-dione and 19 mg (0.47 mmol) of sodium hydroxide in 0.6 mL of D2O was heated at 105° C. for 24 h. The mixture was added to 2 mL of water and acidified with 2N HCl to pH =1. The precipitate was filtered, washed with water, and dried to leave a red solid (19 mg, 80%); mp>360° C.; 1H NMR (DMSO-d6), 7.101 (1, d, J=10.9), 11.10 (mb, 1), 11.70 (mb, 1), 11.99 (s, 1). 1 9F NMR, -137.4 (mb). MS 242 (M+ +1, 100), 195 (50), 152 (20), 140 (25). HRMS, Calcd for C8H4FN3O5 241.0131, found 241.0110

후처리

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. customdried

출처 및 근거

ORD 기록
ord-1cda42afd2c445c796b83e1fe1637bef
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05977107

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