Ammonium Hydroxide → 1-Methyl-7-nitro-3,4-dihydroisoquinoline

HRID 369982

반응식

HRID 369982 반응식
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][N:3]=1.[N+:12]([O-])([O-:14])=[O:13].[K+].[OH-].[NH4+]>>[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=2)[CH2:5][CH2:4][N:3]=1

참가 물질

4

반응물 3

HCID 14923Ammonium HydroxideHCID 24434Potassium NitrateHCID 2315021-Methyl-3,4-dihydroisoquinoline

생성물 1

HCID 109322281-Methyl-7-nitro-3,4-dihydroisoquinoline

실험 절차

1-Methyl-3,4-dihydroisoquinoline (4.25 g, 29.3 mmol) was dissolved in ice cold concentrated sulfuric acid (15 ml) and to this was added potassium nitrate (3.25 g, 32.2 mmol) portionwise with cooling. The mixture was stirred overnight, poured over ice, basified with concentrated ammonium hydroxide, and the precipitated solid was collected, washed with water and dried: 4.47 g (80%), MS (M+H)+ 191, 1H NMR (D2O), 8.30 (d, 1H), 8.22 (dd, 1H), 7.39 (d, 1H), 3.80-3.62 (m, 2H), 2.92-2.70 (m, 2H), 2.48 (broad s, 3H).

후처리

  1. temperaturewith cooling
  2. additionpoured over ice
  3. customthe precipitated solid was collected
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-5cffc12037354434a37b3a773f26cd97
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06140322

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