Hydrochloric Acid → HCID 19038100、化合物

HRID 263457ノート

反応式

HRID 263457 の反応式
[Cl:1][C:2]1[C:3]([O:13][CH:14]2[CH:19]3[CH2:20][CH2:21][N:16]([CH2:17][CH2:18]3)[CH2:15]2)=[N:4][O:5][C:6]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl>C(O)C.O1CCOCC1>[ClH:1].[Cl:1][C:2]1[C:3]([O:13][CH:14]2[CH:19]3[CH2:20][CH2:21][N:16]([CH2:17][CH2:18]3)[CH2:15]2)=[N:4][O:5][C:6]=1[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 19038078HCID 19038078、化合物

生成物 1

HCID 19038100HCID 19038100、化合物収率 198%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 2.12 g of 4-chloro-3-(3-quinuclidinyloxy)-5-phenylisoxazole (prepared as described in Example 9) in 20 ml of ethanol was cooled to 5° C. 2.1 ml of a 4N solution of hydrogen chloride in dioxane were then added dropwise to the solution, and the resulting mixture was stirred at room temperature for 30 minutes. At the end of this time, the reaction mixture was concentrated by distillation under reduced pressure and the solid residue thus obtained was recrystallized from ethanol to afford 2.35 g (yield 96.1%) of the title compound as a colorless powder, melting at 235°-237° C. (with decomposition).

後処理

  1. concentrationAt the end of this time, the reaction mixture was concentrated by distillation under reduced pressure
  2. customthe solid residue thus obtained
  3. customwas recrystallized from ethanol

出典と根拠

ORDレコード
ord-ce77b1584baa49bebc9421e59846f3e6
出典データセット
uspto-grants-1997_07
特許番号
US05643923

反応ノート

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