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Hydrochloric Acid → HCID 20339406, 화합물

HRID 1395453
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HRID 1395453 반응식
Cl.[CH2:2]1[N:7]2[C:8]3[C:13]([NH:14][C:15](=[O:16])[CH:6]2[CH2:5][NH:4][CH2:3]1)=[CH:12][CH:11]=[CH:10][CH:9]=3.[N:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][CH2:25][CH2:26]Cl)=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].Cl>C(O)C.CC(C)=O.C(N(CC)CC)C>[N:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][CH2:25][CH2:26][N:4]2[CH2:3][CH2:2][N:7]3[C:8]4[C:13]([NH:14][C:15](=[O:16])[CH:6]3[CH2:5]2)=[CH:12][CH:11]=[CH:10][CH:9]=4)=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 109539414-(4-Chlorobutyl)pyridineHCID 18377410HCID 18377410, 화합물

생성물 1

HCID 20339406HCID 20339406, 화합물

시약·촉매·용매 3

HCID 180
Acetone
용매
HCID 702Ethanol용매
HCID 8471Triethylamine용매

실험 절차

A solution of 6.2 g. (0.03 mole) of 2,3,4,4a-tetrahydro-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, hydrochloride, 7 g. (0.04 mole) of 4-(4-pyridyl)-1-chlorobutane, 10 g. of potassium carbonate, 5 g. of potassium iodide and 0.5 ml. of triethylamine was stirred and refluxed in 200 ml. of acetone for 48 hours, cooled and filtered. The solvent was removed and the residue was dissolved in methylene chloride. This solution was washed with water and brine, dried over magnesium sulfate and filtered. The solvent was removed and the residue was chromatographed on 500 g. of Silicar, CC-7. Fractions eluted with 10% methanol in ethyl acetate afforded 3.2 g. of free base. 3 G. of the above free base was dissolved in ethanol and treated with dry hydrogen chloride saturated ether. The product hydrochloride was filtered and recrystallized from methanol to give 3.2 g. of the title compound as the dihydrochloride salt, m.p. 281°-283° C.

후처리

  1. temperaturerefluxed in 200 ml
  2. temperaturecooled
  3. filtrationfiltered
  4. customThe solvent was removed
  5. dissolutionthe residue was dissolved in methylene chloride
  6. washThis solution was washed with water and brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customThe solvent was removed
  10. customthe residue was chromatographed on 500 g
  11. washFractions eluted with 10% methanol in ethyl acetate
  12. customafforded 3.2 g
  13. filtrationThe product hydrochloride was filtered
  14. customrecrystallized from methanol
  15. customto give 3.2 g

출처 및 근거

ORD 기록
ord-9519b5cb1e74496091edb226acc00108
출처 데이터셋
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04203987

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