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Hydrochloric Acid → HCID 20339406、化合物

HRID 1395453
ノート
印刷プレビュー

反応式

HRID 1395453 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 109539414-(4-Chlorobutyl)pyridineHCID 18377410HCID 18377410、化合物

生成物 1

HCID 20339406HCID 20339406、化合物

試薬・触媒・溶媒 3

HCID 180
Acetone
溶媒
HCID 702Ethanol溶媒
HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9519b5cb1e74496091edb226acc00108
出典データセット
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04203987

反応ノート

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