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

HRID 263459
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HRID 263459 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c5107a3f6a814cd9816fcb7310da315e
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05643923

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