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

HRID 370903ノート

反応式

HRID 370903 の反応式
[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]

参加物

8

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

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°.

後処理

  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)

出典と根拠

ORDレコード
ord-c6527b948d67408287c11ad14338afa3
出典データセット
uspto-grants-1985_07
特許番号
US04528376

反応ノート

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