Hydrochloric Acid → HCID 15227821, 화합물

HRID 1742526노트

반응식

HRID 1742526 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:13]=[C:12]([C:14](=[O:17])[CH2:15][CH3:16])[O:11][N:10]=2)=[CH:5][CH:4]=1.[CH2:18]=O.[NH:20]1[CH2:24][CH2:23][CH2:22][CH2:21]1.Cl>C(OCC)C.O.ClCCl.C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:13]=[C:12]([C:14](=[O:17])[CH:15]([CH3:18])[CH2:16][N:20]3[CH2:24][CH2:23][CH2:22][CH2:21]3)[O:11][N:10]=2)=[CH:7][CH:8]=1

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 31268PyrrolidineHCID 19976958HCID 19976958, 화합물

생성물 1

HCID 15227821HCID 15227821, 화합물

시약·촉매·용매 4

HCID 702Ethanol용매HCID 962Water용매HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

Added to a mixed solvent of 22 ml of ethyl alcohol and 5 ml of dichloromethane were 2.22 g (9.61 mmol) of 3-(4-methoxyphenyl)-5-propionylisoxazole, 0.96 ml of a 37% aqueous formaldehyde solution and 1.37 g (19.2 mmol) of pyrrolidine, followed by stirring at room temperature for 8 hours. Water and ethyl ether were added, and the resultant mixture was acidified with 2N-hydrochloric acid. The water layer was separated and collected. After the water layer was alkalinized with an aqueous solution of pottasium hydroxide, dichloromethane was added for extraction. The solvent was distilled off, whereby 3-(4-methoxyphenyl)-5-{2-methyl-3-(1-pyrrolidinyl)propionyl} isoxazole was obtained as colorless crystals. Analytical results of the crystals obtained: Yield: 1.73 g (57%). Melting point: 75°-77° C.

후처리

  1. customThe water layer was separated
  2. customcollected
  3. additionwas added for extraction
  4. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-aec6e4076050498c84ef83e68eafb2bb
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05338857

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