Hydrochloric Acid → 3-(1-Allyl-4-piperidyl)-1,2-benzisoxazole hydrochloride

HRID 2417723노트

반응식

HRID 2417723 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([C:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[O:9][N:8]=2)[CH2:3][CH2:2]1.[CH2:16](Br)[CH:17]=[CH2:18].C(=O)(O)[O-].[Na+].[I-].[K+].[ClH:27]>CN(C)C=O.CCOCC>[ClH:27].[CH2:18]([N:1]1[CH2:2][CH2:3][CH:4]([C:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[O:9][N:8]=2)[CH2:5][CH2:6]1)[CH:17]=[CH2:16]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 7841Allyl bromideHCID 516892Sodium BicarbonateHCID 130764363-(Piperidin-4-yl)benzo[d]isoxazole

생성물 1

HCID 130764513-(1-Allyl-4-piperidyl)-1,2-benzisoxazole hydrochloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

A suspension of 4.0 g of 3-(4-piperidyl)-1,2-benzisoxazole, 2.6 g of allyl bromide, 5.0 g of sodium bicarbonate, and 3.0 g of potassium iodide in 90 ml of dimethylformamide was stirred at 80° for 20 hrs. The reaction was cooled, filtered and poured into 1 l of water. The mixture was extracted with ether (three times) and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to give an oil. The oil was dissolved in a small amount of ether into which hydrochloric acid was bubbled. The precipitate was recrystallized from ethanol-ether (three times) to give 2.4 g of product, mp, 174°-176°.

후처리

  1. temperatureThe reaction was cooled
  2. filtrationfiltered
  3. additionpoured into 1 l of water
  4. extractionThe mixture was extracted with ether (three times)
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customto give an oil
  8. customwas bubbled
  9. customThe precipitate was recrystallized from ethanol-ether (three times)

출처 및 근거

ORD 기록
ord-49a8eb664c4c4b2fbf2b81919796b152
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04469869

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