Sodium Sulfate → 8-Bromo-6-methoxyisoquinoline

HRID 2069081ノート

反応式

HRID 2069081 の反応式
S([O-])([O-])(=O)=O.[Na+].[Na+].[Br:8][C:9]1[CH:10]=[C:11]([O:19][CH3:20])[CH:12]=[C:13]2[C:18]=1[CH2:17][NH:16][CH2:15][CH2:14]2>[O-2].[O-2].[Mn+4].C1(C)C=CC=CC=1>[Br:8][C:9]1[CH:10]=[C:11]([O:19][CH3:20])[CH:12]=[C:13]2[C:18]=1[CH:17]=[N:16][CH:15]=[CH:14]2

参加物

5

反応物 2

HCID 24436Sodium SulfateHCID 674039748-Bromo-6-methoxy-1,2,3,4-tetrahydroisoquinoline

生成物 1

HCID 595347478-Bromo-6-methoxyisoquinoline収率 35.7%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 1140Toluene溶媒

反応条件

温度
140 °C

実験手順

Sodium sulfate (2.8 g) and manganese dioxide (7.1 g; Ald) were added to a toluene (60 mL) solution of Intermediate 5 (1.99 g) and the resulting mixture was stirred at 140° C. for 24 hours. The reaction mixture was filtrated through celite followed by the addition of 2 N hydrochloric acid and the resulting mixture was washed with ether. The resulting mixture was neutralized with 5 N aqueous sodium hydroxide solution and then extracted with dichloromethane to give the title compound (698 mg).

後処理

  1. filtrationThe reaction mixture was filtrated through celite
  2. additionfollowed by the addition of 2 N hydrochloric acid
  3. washthe resulting mixture was washed with ether
  4. extractionextracted with dichloromethane

出典と根拠

ORDレコード
ord-3e8e20bb7d444874a7b463aec3541926
出典データセット
uspto-grants-2012_10
特許番号
US08299055B2

反応ノート

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