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

HRID 369982

反応式

HRID 369982 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-5cffc12037354434a37b3a773f26cd97
出典データセット
uspto-grants-2000_10
特許番号
US06140322

関連ノート

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