Hydrochloric Acid → HCID 19976901, 화합물

HRID 1742529노트

반응식

HRID 1742529 반응식
[CH2:1]([C:8]1[CH:12]=[C:11]([C:13](=[O:16])[CH2:14][CH3:15])[O:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:17].[NH:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.[CH2:24]=O.Cl>O1CCOCC1.C(OCC)C>[ClH:17].[CH2:1]([C:8]1[CH:12]=[C:11]([C:13](=[O:16])[CH:14]([CH3:24])[CH2:15][N:18]2[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]2)[O:10][N:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 2723721Piperidine, hydrochloride (1:1)HCID 19976952HCID 19976952, 화합물

생성물 1

HCID 19976901HCID 19976901, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매

실험 절차

In 2 ml of dioxane, 1.5 g (7 mmol) of 3-benzyl-5-propionylisoxazole prepared above in the procedure (2), 0.93 g (7.7 mmol) of piperidine hydrochloride, 0.25 g (8.3 mmol) of paraformaldehyde and two droplets of 12N-hydrochloric acid were heated under reflux for 60 minutes. When left over in a cool place for 3 days after completion of the reaction, the reaction mixture became a solid. Diethyl ether was added to the solid. A solid was collected by filtration and then dried, whereby 3-benzyl-5-(2-methyl-3-piperidinopropionyl)isoxazole hydrochloride was obtained as colorless crystals. Analytical results of the crystals obtained: Yield: 1.6 g (73.5%).

후처리

  1. temperaturewere heated
  2. temperatureunder reflux for 60 minutes
  3. customafter completion of the reaction
  4. filtrationA solid was collected by filtration
  5. customdried

출처 및 근거

ORD 기록
ord-3cf670fb5d7d4c1c83c197b0ff5bf197
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05338857

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