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Hydrochloric Acid → 1-(4-Bromophenyl)piperidin-4-one

HRID 715559
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인쇄 미리보기

반응식

HRID 715559 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.Cl.[OH-].[Na+]>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:9][CH2:10][C:11](=[O:12])[CH2:16][CH2:17]2)=[CH:4][CH:3]=1
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참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 121693418-(4-Bromophenyl)-1,4-dioxa-8-azaspiro[4.5]decane

생성물 1

HCID 246921481-(4-Bromophenyl)piperidin-4-one

반응 조건

온도
50 °C

실험 절차

A mixture of 8-(4-bromophenyl)-1,4-dioxa-8-azaspiro[4.5]decane (1.02 g) and half concentrated hydrochloric acid is heated for 12 hours at 50° C., poured on ice and aqueous NaOH solution (4 M) is added until pH ˜7-8. Then the mixture is extracted with ethylacetate and the organic phase is washed with brine and dried (MgSO4). The solvents are evaporated in vacuo to give the title compound. LC (method 2): tR=0.96 min; Mass spectrum (ESI+): m/z=254 [M+H]+.

후처리

  1. additionis added until pH ˜7-8
  2. extractionThen the mixture is extracted with ethylacetate
  3. washthe organic phase is washed with brine
  4. dry with materialdried (MgSO4)
  5. customThe solvents are evaporated in vacuo

출처 및 근거

ORD 기록
ord-e6f97f668b9f407bb0e96ca54852e611
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187477B2

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