Water → HCID 21990198, 화합물

HRID 857864

반응식

HRID 857864 반응식
[N:1]1[CH:2]=[CH:3][N:4]2[C:13]=1[CH2:12][C:11]1[CH:10]=[C:9](O)[C:8]([OH:15])=[CH:7][C:6]=1[CH2:5]2.[C:16]([O-:19])([O-])=O.[K+].[K+].O.[CH3:23]N(C=O)C>[Cl-].C1([N+](C)(C)C)C=CC=CC=1>[CH3:23][O:15][C:8]1[C:9]([O:19][CH3:16])=[CH:10][C:11]2[CH2:12][C:13]3[N:4]([CH:3]=[CH:2][N:1]=3)[CH2:5][C:6]=2[CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 219902425,10-Dihydroimidazo[1,2-b]isoquinoline-7,8-diol

생성물 1

HCID 21990198HCID 21990198, 화합물수율 8.4%

시약·촉매·용매 1

HCID 67309Phenyltrimethylammonium chloride촉매

실험 절차

A mixture of 5,10-dihydro-imidazo[1,2-b]isoquinoline-7,8-diol, obtained according to the procedure described in Ex.No. A8c, (0.155 mol), phenyltrimethylammonium chloride (0.31 mol) and K2CO3 (0.68 mol) in DMF (400 ml) was stirred at 90° C. for 20 hours, cooled, poured out into H2O and filtered over dicalite. The filtrate was separated into its layers. The organic layer was washed with H2O, dried (MgSO4), filtered and the solvent was evaporated. The residue was purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 100/0 to 97/3). The pure fractions were collected and the solvent was evaporated, yielding 3 g of 5,10-dihydro-7,8-dimethoxyimidazo[1,2-b]isoquinoline (8.4%) (interm. 22).

후처리

  1. customobtained
  2. temperaturecooled
  3. filtrationfiltered over dicalite
  4. customThe filtrate was separated into its layers
  5. washThe organic layer was washed with H2O
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent was evaporated
  9. customThe residue was purified over silica gel on a glass
  10. filtrationfilter (eluent: CH2Cl2/CH3OH 100/0 to 97/3)
  11. customThe pure fractions were collected
  12. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-bdb3d2557df3483ea49c1d79a50094d8
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07148214B1

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