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Hydrochloric Acid → HCID 69115392, 화합물

HRID 2054168
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HRID 2054168 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])=[CH:4][C:3]=1[CH:19]1[CH2:24][CH2:23][N:22](C(OC(C)(C)C)=O)[CH2:21][CH2:20]1.Cl>C(Cl)Cl>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])=[CH:4][C:3]=1[CH:19]1[CH2:20][CH2:21][NH:22][CH2:23][CH2:24]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 69115646HCID 69115646, 화합물

생성물 1

HCID 69115392HCID 69115392, 화합물수율 98.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

tert-Butyl 4-{2-methyl-5-[(phenylmethoxy)carbonylamino]phenyl}piperidine carboxylate (7.50 g, 17.6 mmol) was dissolved in CH2Cl2 (120 mL) and a HCl solution (4M in dioxane, 52.0 mL) was added and stirred for 1 h. The mixture was concentrated in vacuo and redissolved in CH2Cl2. Aqueous Na2CO3 solution (1 M) was added and the biphasic mixture was stirred for 20 min and separated. The organic layer was further washed with water, dried over Na2SO4 and concentrated in vacuo to afford N-(4-methyl-3-(4-piperidyl)phenyl)(phenylmethoxy)carboxamide (5.61 g, 98% yield) as a white solid. ESMS m/e: 326.0 (M+H)+.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. dissolutionredissolved in CH2Cl2
  3. additionAqueous Na2CO3 solution (1 M) was added
  4. stirringthe biphasic mixture was stirred for 20 min
  5. customseparated
  6. washThe organic layer was further washed with water
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-091e5278c786411d871a9fd5573ffdcc
출처 데이터셋
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07329656B2

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