Potassium Carbonate → HCID 10361909, 화합물

HRID 1451632노트

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HRID 1451632 반응식
Br[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1.Cl.[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][C:27]=1[O:28][CH3:29])[CH2:24][NH:23][CH2:22][CH2:21]2.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][C:27]=1[O:28][CH3:29])[CH2:24][N:23]([CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1)[CH2:22][CH2:21]2

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2611281-(3-Bromopropoxy)-4-nitrobenzeneHCID 64560356,7-Dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrochloride

생성물 1

HCID 10361909HCID 10361909, 화합물수율 79.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1-(3-bromopropoxy)-4-nitrobenzene (10 g), 1,2,3,4-tetrahydro-6,7-dimethoxyisoquinoline hydrochloride (8.8 g) and potassium carbonate (10.6 g) in DMF (100 ml) was heated at 100° for 16 h. The mixture was then filtered and the filtrate evaporated. The residue was taken up in water and extracted with dichloromethane. The organic layer was washed with water, dried, and evaporated to give an oil which crystallised in ether to give the title compound (11.3 g), m.p. 100°.

후처리

  1. temperaturewas heated at 100° for 16 h
  2. filtrationThe mixture was then filtered
  3. customthe filtrate evaporated
  4. extractionextracted with dichloromethane
  5. washThe organic layer was washed with water
  6. customdried
  7. customevaporated
  8. customto give an oil which
  9. customcrystallised in ether

출처 및 근거

ORD 기록
ord-ca46219a13b54da39dd6280e340590a1
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05604237

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