Water → HCID 22499375, 화합물

HRID 1989861노트

반응식

HRID 1989861 반응식
Cl.[C:2]1([CH:8]([CH:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[C:9]#[N:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.F[C:18]1[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[N+:24]([C:21]1[CH:22]=[CH:23][C:18]([N:14]2[CH2:15][CH2:16][CH:11]([CH:8]([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:9]#[N:10])[CH2:12][CH2:13]2)=[CH:19][CH:20]=1)([O-:26])=[O:25]

참가 물질

6

반응물 4

HCID 962WaterHCID 9590p-FluoronitrobenzeneHCID 11430Potassium CarbonateHCID 222528504-Piperidineacetonitrile, α-phenyl-, hydrochloride (1:1)

생성물 1

HCID 22499375HCID 22499375, 화합물수율 66.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

A mixture of α-phenyl-4-piperidineacetonitrile monohydrochloride (0.05 mol), 1-fluoro-4-nitrobenzene (0.06 mol) and K2CO3 (0.15 mol) in DMF (200 ml) was stirred at 50° C. for 4 hours, cooled, poured out into water and extracted with DCM. The organic layer was separated, washed with water, dried, filtered and the solvent was evaporated. The residue was crystallized from DIPE. The precipitate was filtered off and dried, yielding 10.7 g of (±)-1-(4-nitrophenyl)-α-phenyl-4-piperidineacetonitrile (intermediate 15, mp. 118° C.).

후처리

  1. temperaturecooled
  2. extractionextracted with DCM
  3. customThe organic layer was separated
  4. washwashed with water
  5. customdried
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customThe residue was crystallized from DIPE
  9. filtrationThe precipitate was filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-98bae33066d14d878cd9174e12bf4191
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642378B2

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