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Sodium Hydroxide → HCID 23112486, 화합물

HRID 456555
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HRID 456555 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[C:14]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:19][C:18]=2[F:27])[O:15]C)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CC(C)=O.Cl>[CH2:1]([N:8]1[CH2:9][CH2:10][CH:11]([C:14]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:24])[F:25])=[CH:19][C:18]=2[F:27])=[O:15])[CH2:12][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 58817534HCID 58817534, 화합물

생성물 1

HCID 23112486HCID 23112486, 화합물수율 92.3%

시약·촉매·용매 2

HCID 180Acetone용매HCID 313Hydrochloric Acid용매

실험 절차

A solution of the 1-benzyl-4-[(2-fluoro-4-trifluoromethyl-phenyl)-methoxy-methylene]-piperidine (9.9 g, 26.1 mmol) in acetone (100 mL) and conc. HCl (10 mL) in a sealed vessel was heated at 60° C. for 2 hours. Upon cooling to room temperature the solution was basified with the addition of 3 N NaOH. The resulting mixture was extracted with EtOAc (2×200 mL). The combined extracts were washed with brine (50 mL), dried (MgSO4), filtered and evaporated yielding 8.8 g (92%) of the desired product as a solid.

후처리

  1. extractionThe resulting mixture was extracted with EtOAc (2×200 mL)
  2. washThe combined extracts were washed with brine (50 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-5f6b3b9e6a4f4d199d05cac39dcd0eea
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07186724B2

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