Nitric Acid → HCID 13136924、化合物

HRID 851196ノート

反応式

HRID 851196 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 13136924HCID 13136924、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-64f2da6b926b488bbec66803a14828a1
出典データセット
uspto-grants-1983_05
特許番号
US04382939

反応ノート

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