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Nitric Acid → HCID 19867711, 화합물

HRID 1198946
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HRID 1198946 반응식
S(=O)(=O)(O)O.[CH3:6][C:7]1([CH3:19])[C:16]2[C:11](=[C:12]([CH3:17])[CH:13]=[CH:14][CH:15]=2)[NH:10][C:9](=[O:18])[CH2:8]1.C(=O)([O-])[O-].[Na+].[Na+].[N+:26]([O-])([OH:28])=[O:27]>>[CH3:6][C:7]1([CH3:19])[C:16]2[C:11](=[C:12]([CH3:17])[CH:13]=[C:14]([N+:26]([O-:28])=[O:27])[CH:15]=2)[NH:10][C:9](=[O:18])[CH2:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 944Nitric AcidHCID 1118Sulfuric Acid2회HCID 10340Sodium CarbonateHCID 198677004,4,8-Trimethyl-3,4-dihydroquinolin-2(1H)-one

생성물 1

HCID 19867711HCID 19867711, 화합물

실험 절차

A mixture of concentrated nitric acid (10 cm3, S.G.=1.42) and 98% w/w sulphuric acid (25 cm3) was added dropwise to a stirred solution of 3,4-dihydro-4,4,8-trimethyl-2-(1H)-quinolone (6 g) in 98% w/w sulphuric acid (25 cm3) cooled to -10°. The temperature was maintained at -10° for a further 30 minutes, the mixture poured onto ice (200 g), basified to pH 9 with saturated sodium carbonate solution and extracted with methanol:chloroform, 1:20 by volume (2×300 cm3). The combined and dried (MgSO4) organic extracts were evaporated in vacuo to give the title compound (6.46 g) which was characterised spectroscopically and used directly in Preparation 24 without further purification.

후처리

  1. temperaturecooled to -10°
  2. temperatureThe temperature was maintained at -10° for a further 30 minutes
  3. additionthe mixture poured onto ice (200 g)
  4. extractionextracted with methanol
  5. dry with materialdried (MgSO4) organic extracts
  6. customwere evaporated in vacuo

출처 및 근거

ORD 기록
ord-651a0f33bbf8402c83cdbdee82bca7ef
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04898872

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