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Potassium Nitrate → 4-methyl-7-nitro-3,4-dihydro-2H-isoquinolin-1-one

HRID 1358254
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HRID 1358254 반응식
[CH3:1][CH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5](=[O:12])[NH:4][CH2:3]1.[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[CH3:1][CH:2]1[C:11]2[C:6](=[CH:7][C:8]([N+:13]([O-:15])=[O:14])=[CH:9][CH:10]=2)[C:5](=[O:12])[NH:4][CH2:3]1
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참가 물질

4

반응물 2

HCID 24434Potassium NitrateHCID 140400954-Methyl-3,4-dihydroisoquinolin-1(2H)-one

생성물 1

HCID 181844524-methyl-7-nitro-3,4-dihydro-2H-isoquinolin-1-one

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

A solution of 4-methyl-3,4-dihydro-2H-isoquinolin-1-one (1. Og) (J. Med. Chem., 1988, 31, 433) in conc. sulfuric acid (5 ml) was added dropwise over 20 min to an ice cooled solution of potassium nitrate (0.678 g) in conc. sulfuric acid (5 ml). The mixture was stirred for a further 30 min with ice-cooling. The mixture was added dropwise to ice (150 g) with stirring. The precipitated solid was collected by filtration, washed with water and dried to give the sub-titl compound (0.95 g). 1H NMR δ: 1.28 (3H, d, J=6.6 Hz), 3.14-3.28 (1H, m), 3.52 (2H, m), 7.67 (1H, d, J=8.5 Hz), 8.29 (1H, s), 8.35 (1H, dd, J=2.5, 8.4 Hz) (1H, d, J=2.5 Hz).

후처리

  1. temperaturecooling
  2. stirringwith stirring
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-2c4296ca823b4d7698a6f584b768aea2
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06596730B1

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