Hydrochloric Acid → HCID 19976901、化合物

HRID 1440325ノート

反応式

HRID 1440325 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 2723721Piperidine, hydrochloride (1:1)HCID 19976952HCID 19976952、化合物

生成物 1

HCID 19976901HCID 19976901、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3265bfb670bc40aeb0a0006974b19fca
出典データセット
uspto-grants-1996_03
特許番号
US05498619

反応ノート

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