Potassium Carbonate → HCID 15745003, 화합물

HRID 327442노트

반응식

HRID 327442 반응식
[CH2:1]([NH:4][CH:5]1[CH2:14][C:13]2=[CH:15][CH:16]=[CH:17][C:11]3=[C:12]2[N:7]([CH2:8][CH2:9][CH2:10]3)[CH2:6]1)[CH2:2][CH3:3].[CH2:18](I)[CH2:19][CH3:20].C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+]>CN(C)C=O.C(OCC)(=O)C>[CH2:1]([N:4]([CH2:18][CH2:19][CH3:20])[CH:5]1[CH2:14][C:13]2=[CH:15][CH:16]=[CH:17][C:11]3=[C:12]2[N:7]([CH2:8][CH2:9][CH2:10]3)[CH2:6]1)[CH2:2][CH3:3]

참가 물질

7

반응물 4

HCID 11430Potassium Carbonate2회HCID 14798Sodium HydroxideHCID 336431-Iodopropane2회HCID 15745002HCID 15745002, 화합물

생성물 1

HCID 15745003HCID 15745003, 화합물수율 80.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

A mixture of 2,3,6,7-tetrahydro-N-propyl-1H,5H-benzo(ij)quinolizin-2-amine (2.33 g, 0.01 mol), propyl iodide (5.16 g, 0.03 mol) and anhydrous potassium carbonate (3 g, 0.02 mol) in dimethylformamide (75 mL) was stirred for 5 hours at 90° C. At this time additional propyl iodide (1.72 g, 0.01 mol) and potassium carbonate (0.05 g, 0.0036 mol) were added and the reaction was continued for an additional 2 hours. The reaction was cooled, filtered to remove inorganic material, and the solvent was removed under reduced pressure. The product was partitioned between ethyl acetate (800 mL) and 4N sodium hydroxide (20 mL, 0.08 mol), the organic layer concentrated, filtered, and chromatographed on silica gel in 5-30% ethyl acetate:hexane to give 2.19 g of 2,3,6,7-tetrahydro-N,N-dipropyl-1H,5H-benzo(ij)quinolizin-2-amine.

후처리

  1. waitthe reaction was continued for an additional 2 hours
  2. temperatureThe reaction was cooled
  3. filtrationfiltered
  4. customto remove inorganic material
  5. customthe solvent was removed under reduced pressure
  6. concentrationthe organic layer concentrated
  7. filtrationfiltered
  8. customchromatographed on silica gel in 5-30% ethyl acetate

출처 및 근거

ORD 기록
ord-6245e626f77a43ca953bcd15e3f03f40
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05273975

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