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1,4-Dioxane hydrochloride → 4-{1-(4-fluorophenyl)-2-[4-(4-naphthalen-1-yl-butyl)piperazin-1-yl]-2-oxoethyl}-1-methyl-3,6-dihydro-2H-pyridine

HRID 497346
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HRID 497346 반응식
C(O[C:6]([N:8]1[CH2:13][CH:12]=[C:11]([CH:14]([C:37]2[CH:42]=[CH:41][C:40]([F:43])=[CH:39][CH:38]=2)[C:15]([N:17]2[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][CH2:25][CH2:26][C:27]3[C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[CH:29][CH:28]=3)[CH2:19][CH2:18]2)=[O:16])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.O1CCOCC1>CO>[F:43][C:40]1[CH:39]=[CH:38][C:37]([CH:14]([C:11]2[CH2:12][CH2:13][N:8]([CH3:6])[CH2:9][CH:10]=2)[C:15]([N:17]2[CH2:18][CH2:19][N:20]([CH2:23][CH2:24][CH2:25][CH2:26][C:27]3[C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[CH:29][CH:28]=3)[CH2:21][CH2:22]2)=[O:16])=[CH:42][CH:41]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 223186421-t-butoxycarbonyl-4-{1-(4-fluorophenyl)-2-[4-(4-naphthalen-1-yl-butyl)piperazin-1-yl]-2-oxoethyl}-3,6-dihydro-2H-pyridine

생성물 1

HCID 223186454-{1-(4-fluorophenyl)-2-[4-(4-naphthalen-1-yl-butyl)piperazin-1-yl]-2-oxoethyl}-1-methyl-3,6-dihydro-2H-pyridine수율 59.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

0.49 g of 1-t-Butoxycarbonyl-4-{1-(4-fluorophenyl)-2-[4-(4-naphthalen-1-yl-butyl)piperazin-1-yl]-2-oxoethyl}-3,6-dihydro-2H-pyridine was dissolved in 5 ml of methanol, and 20 ml of 4M hydrogen chloride/1,4-dioxane solution was added, followed by stirring at room temperature for 2 hours. The reaction solution was concentrated under reduced pressure, ethyl acetate was added to the residue, the mixture was washed with 1M aqueous sodium hydroxide solution and a saturated aqueous sodium solution. The organic layer was dried over anhydrous sodium sulfate. After removal of the drying agent by filtration, the filtrate was concentrated under reduced pressure. The residue was dissolved in 5 ml of acetonitrile, and 340 μl of 37% formalin, 200 μl of acetic acid and 90 mg of sodium cyanoborohydride were added, followed by stirring at room temperature for an hour. The reaction solution was diluted with ethyl acetate and washed with a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous sodium sulfate. After removal of the drying agent by filtration, the filtrate was concentrated under reduced pressure. The residue was purified by a silica gel column chromatography (Chromatorex NH, hexane:ethyl acetate=2:1) to give 0.25 g of 4-{1-(4-fluorophenyl)-2-[4-(4-naphthalen-1-yl-butyl)piperazin-1-yl]-2-oxoethyl}-1-methyl-3,6-dihydro-2H-pyridine as an oil.

후처리

  1. concentrationThe reaction solution was concentrated under reduced pressure, ethyl acetate
  2. additionwas added to the residue
  3. washthe mixture was washed with 1M aqueous sodium hydroxide solution
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customAfter removal of the drying agent
  6. filtrationby filtration
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. dissolutionThe residue was dissolved in 5 ml of acetonitrile
  9. addition340 μl of 37% formalin, 200 μl of acetic acid and 90 mg of sodium cyanoborohydride were added
  10. stirringby stirring at room temperature for an hour
  11. additionThe reaction solution was diluted with ethyl acetate
  12. washwashed with a saturated aqueous sodium bicarbonate solution
  13. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  14. customAfter removal of the drying agent
  15. filtrationby filtration
  16. concentrationthe filtrate was concentrated under reduced pressure
  17. customThe residue was purified by a silica gel column chromatography (Chromatorex NH, hexane:ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-cf31b82e56eb4a28bc225cada343f2dd
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06949552B2

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