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Hydrochloric Acid → 5-Chloro-3-(1-methyl-4-piperidyloxy)-1,2-benzisoxazole hydrochloride

HRID 263459
ノート
印刷プレビュー

反応式

HRID 263459 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH:11]3[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]3)[C:6]=2[CH:18]=1.Cl>C(O)C.O1CCOCC1>[ClH:1].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH:11]3[CH2:12][CH2:13][N:14]([CH3:17])[CH2:15][CH2:16]3)[C:6]=2[CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 190380875-Chloro-3-(1-methyl-4-piperidyloxy)-1,2-benzisoxazole

生成物 1

HCID 190381165-Chloro-3-(1-methyl-4-piperidyloxy)-1,2-benzisoxazole hydrochloride収率 197.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 2.20 g (8.24 mmole) of 5-chloro-3-(1-methyl-4-piperidyloxy)-1,2-benzisoxazole (prepared as described in Example 11) in 20 ml of ethanol was cooled to 5° C. 2.5 ml of a 4N solution of hydrogen chloride in dioxane were added dropwise to the cooled solution, and the resulting mixture was stirred at room temperature for 30 minutes. At the end of this time, the solvent was removed from the reaction mixture by distillation under reduced pressure. The solid residue thus obtained was recrystallized from ethanol to afford 2.47 g (yield 98.7%) of the title compound as colorless curd-like crystals, melting at 212°-214° C. (with decomposition).

後処理

  1. customAt the end of this time, the solvent was removed from the reaction mixture 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-c5107a3f6a814cd9816fcb7310da315e
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05643923

反応ノート

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