Nitric Acid → HCID 21877762, 화합물

HRID 723911노트

반응식

HRID 723911 반응식
[F:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2.[N+:13]([O-])([OH:15])=[O:14]>S(=O)(=O)(O)O>[F:1][C:2]1[CH:3]=[C:4]([N+:13]([O-:15])=[O:14])[CH:5]=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 151448738-Fluoro-1,2,3,4-tetrahydroquinolin-2-one

생성물 1

HCID 21877762HCID 21877762, 화합물수율 75%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
-5 °C

실험 절차

8-Fluoro-3,4-dihydro-1H-quinolin-2-one [prepared according to the procedure found in EP0524846] (2.62 g, 0.0159 mol) is dissolved in concentrated sulfuric acid (20 ml) and cooled to −5° C. Nitric acid (70%, 1.02 ml, 0.0159 mol) is added dropwise and the reaction stirred at −5° C. for 20 minutes. The mixture is poured onto ice and the resulting precipitate collected by filtration, washed well with water, and dried under vacuum. Purification by flash column chromatography (30% ethyl acetate/hexane) gives the title compound as a light yellow solid (2.50 g, 75%); [M+H]+=211.

후처리

  1. additionThe mixture is poured onto ice
  2. filtrationthe resulting precipitate collected by filtration
  3. washwashed well with water
  4. customdried under vacuum
  5. customPurification by flash column chromatography (30% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-f9ecd6c29b8d46df9d067d2acfbefb4d
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141588B2

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