Sodium Sulfate → 8-Bromo-6-methoxyisoquinoline

HRID 2069081노트

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HRID 2069081 반응식
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

참가 물질

5

반응물 2

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

생성물 1

HCID 595347478-Bromo-6-methoxyisoquinoline수율 35.7%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 1140Toluene용매

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온도
140 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3e8e20bb7d444874a7b463aec3541926
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299055B2

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