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Hydrochloric Acid → HCID 20339412, 화합물

HRID 1395449
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HRID 1395449 반응식
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]1[CH2:13][CH2:14][NH:15][CH2:16][CH:8]1[C:7](=[O:17])[NH:6]2.[CH:20]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)=[CH2:21].CO.Cl>C(O)C.C(O)(=O)C>[N:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[CH2:20][CH2:21][N:15]1[CH2:14][CH2:13][N:9]2[C:10]3[C:5]([NH:6][C:7](=[O:17])[CH:8]2[CH2:16]1)=[CH:4][C:3]([C:2]([F:18])([F:1])[F:19])=[CH:12][CH:11]=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 75212-VinylpyridineHCID 203394142,3,4,4a-Tetrahydro-8-(trifluoromethyl)-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one

생성물 1

HCID 20339412HCID 20339412, 화합물수율 71%

시약·촉매·용매 2

HCID 176Acetic Acid
용매
HCID 702Ethanol용매

실험 절차

A solution of 8.5 g. (0.03 mole) of 2,3,4,4a-tetrahydro-8-trifluoromethyl-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one and 17.5 g. (0.16 mole) of 2-vinylpyridine in 250 ml. of methanol containing 7 ml. acetic acid was heated under reflux for 20 hours. The reaction mixture was cooled, and the solvent was removed under reduced pressure. The residue was precipitated with 1 l. of water. The product was filtered and recrystallized from methanol-water to yield 10.1 g. of free base. 4.5 G. of this free base was dissolved in 150 ml. of absolute ethanol and treated with dry hydrogen chloride saturated ether solution. The product hydrochloride was filtered and recrystallized two times from methanol-ether to give 4 g. (71%) of the title compound as the dihydrochloride salt, m.p. 194°-196° C.

후처리

  1. temperatureunder reflux for 20 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent was removed under reduced pressure
  4. customThe residue was precipitated with 1 l
  5. filtrationThe product was filtered
  6. customrecrystallized from methanol-water
  7. customto yield 10.1 g
  8. dissolutionof this free base was dissolved in 150 ml
  9. filtrationThe product hydrochloride was filtered
  10. customrecrystallized two times from methanol-ether
  11. customto give 4 g

출처 및 근거

ORD 기록
ord-957a35fd298a4cc28c3e29bf5720b8a3
출처 데이터셋
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04203987

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