Methyl iodide → HCID 20039734, 화합물

HRID 1762809노트

반응식

HRID 1762809 반응식
[CH:1]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:2]=1[CH2:3][C:4]1[N:5]([CH:11]=[C:12]3[C:17]=1[C:16](=[O:18])[C:15]1[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=1[C:13]3=[O:23])[CH2:6]2.[C:24](=O)([O-])[O-].[K+].[K+].IC>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C(#N)C.ClCCl>[CH3:24][CH:3]1[C:2]2[C:7](=[CH:8][CH:9]=[CH:10][CH:1]=2)[CH2:6][N:5]2[CH:11]=[C:12]3[C:17]([C:16](=[O:18])[C:15]4[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=4[C:13]3=[O:23])=[C:4]12

참가 물질

7

반응물 3

HCID 6328Methyl iodide2회HCID 11430Potassium CarbonateHCID 71772Mitoquidone2회

생성물 1

HCID 20039734HCID 20039734, 화합물수율 9.8%

시약·촉매·용매 3

HCID 66133Benzyl triethylammonium chloride촉매HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 5,14-dihydrobenz[5,6]isoindolo[2,1-b]isoquinoline-8,13-dione (0.96 g) (Intermediate 1), benzyl triethylammonium chloride (0.16 g), potassium carbonate (2.20 g) and iodomethane (0.45 ml) in acetonitrile (100 ml) was stirred and heated under reflux for 4 h. A further portion of iodomethane (0.5 ml) was added and the mixture was stirred at 80° C. for 1 h. The mixture was cooled to room temperature, diluted with dichloromethane (250 ml) and filtered. The filtrate was concentrated in vacuo and the residue was purified on preparative plates eluting five times with chloroform to give the title compound (98 mg) m.p. 215°-218° C. λmax (in CHCl3) 246.5 nm (ε51,050), 266.5 nm (ε18,250) and 366.55 nm (ε3,700).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 4 h
  3. stirringthe mixture was stirred at 80° C. for 1 h
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue was purified on preparative plates
  7. washeluting five times with chloroform

출처 및 근거

ORD 기록
ord-840537cf7f7a408c894e6692af625f16
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835158

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