Cesium fluoride → HCID 22498336, 화합물

HRID 984503노트

반응식

HRID 984503 반응식
[NH:1]1[CH2:13][CH2:12][CH2:11][CH:3]([C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5])[CH2:2]1.F[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N+:21]([O-:23])=[O:22].[F-].[Cs+]>C1(C)C=CC=CC=1.C(OCC)(=O)C>[N+:21]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[N:1]1[CH2:13][CH2:12][CH2:11][CH:3]([C:4]([O:6][C:7]([CH3:9])([CH3:10])[CH3:8])=[O:5])[CH2:2]1)([O-:23])=[O:22]

참가 물질

6

반응물 3

HCID 25953Cesium fluorideHCID 738951-Fluoro-2-nitrobenzeneHCID 42271713-Piperidinecarboxylic acid t-butyl ester HCl

생성물 1

HCID 22498336HCID 22498336, 화합물수율 96.2%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of Example 437C (10.4 g, 56.1 mmol) in toluene (112 mL) was added 2-fluoronitrobenzene (6.0 mL, 56 mmol) and CsF (852 mg, 5.6. mmol). The reaction mixture was stirred under reflux conditions for 18 h, and allowed to cool to ambient temperature. The mixture was diluted with ethyl acetate (100 mL), washed with 10% HCl (2×50 mL), followed by brine (3×100 mL), then dried (Na2SO4) and evaporated in vacuo to obtain the title compound (16.5 g, 94%). MS (ESI) m/e 307 (M+H)+.

후처리

  1. washwashed with 10% HCl (2×50 mL)
  2. dry with materialdried (Na2SO4)
  3. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-19767238f58047c89c8fdb090d7edeb8
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06867203B2

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