Hydrochloric Acid → HCID 15227821、化合物

HRID 1742526ノート

反応式

HRID 1742526 の反応式
[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

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 31268PyrrolidineHCID 19976958HCID 19976958、化合物

生成物 1

HCID 15227821HCID 15227821、化合物

試薬・触媒・溶媒 4

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-aec6e4076050498c84ef83e68eafb2bb
出典データセット
uspto-grants-1994_08
特許番号
US05338857

反応ノート

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