Nitric Acid → HCID 13136924, 화합물

HRID 851196노트

반응식

HRID 851196 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]2[C:8]3[CH2:13][CH2:12][NH:11][CH2:10][C:9]=3[C:14](=[O:16])[O:15][C:4]=2[CH:3]=1.S(=O)(=O)(O)O.[N+:22]([O-])([OH:24])=[O:23]>O>[CH3:1][C:2]1[C:7]([N+:22]([O-:24])=[O:23])=[CH:6][C:5]2[C:8]3[CH2:13][CH2:12][NH:11][CH2:10][C:9]=3[C:14](=[O:16])[O:15][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 106087088-Methyl-1,2,3,4-tetrahydro-chromeno[3,4-c]pyridin-5-one

생성물 1

HCID 13136924HCID 13136924, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A stirred suspension of 1,2,3,4-tetrahydro-8-methyl-5H-[1]benzopyrano[3,4-c]pyridin-5-one (10.0 g, 0.046 moles) in water (10 ml) is cooled in an ice bath. Concentrated sulfuric acid (25 ml) is added, followed after 15 minutes by the dropwise addition of concentrated nitric acid (12 ml). The ice bath is removed and the mixture allowed to warm to room temperature. After 48 hours the mixture is poured over crushed ice, stirred, and made strongly basic by the addition of concentrated ammonium hydroxide. The precipitated product is filtered off, rinsed with water and dried. Recrystallization from acetonitrile gave the product (8.7 g), mp 197°-199° C.

후처리

  1. temperatureis cooled in an ice bath
  2. customThe ice bath is removed
  3. additionAfter 48 hours the mixture is poured
  4. customover crushed ice
  5. additionmade strongly basic by the addition of concentrated ammonium hydroxide
  6. filtrationThe precipitated product is filtered off
  7. washrinsed with water
  8. customdried
  9. customRecrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-64f2da6b926b488bbec66803a14828a1
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04382939

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