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Cesium carbonate → 1,1-Dimethylethyl 4-[(4-nitro-2-pyridinyl)oxy]-1-piperidinecarboxylate

HRID 1993664
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HRID 1993664 반응식
Cl[C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][N:3]=1.[OH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]1.C(=O)([O-])[O-].[Cs+].[Cs+].C(P(C(C)(C)C)C1C=CC2C(=CC=CC=2)C=1C1C2C(=CC=CC=2)C=CC=1)(C)(C)C>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(C)C=CC=CC=1>[C:21]([O:20][C:18]([N:15]1[CH2:16][CH2:17][CH:12]([O:11][C:2]2[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][N:3]=2)[CH2:13][CH2:14]1)=[O:19])([CH3:24])([CH3:22])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 643502Tert-butyl 4-hydroxypiperidine-1-carboxylateHCID 7351522-Chloro-4-nitropyridineHCID 2734941(1,1'-Binaphthalen)-2-yldi-tert-butylphosphine

생성물 1

HCID 685380211,1-Dimethylethyl 4-[(4-nitro-2-pyridinyl)oxy]-1-piperidinecarboxylate

시약·촉매·용매 2

HCID 167845
palladium(II) acetate
촉매
HCID 1140Toluene용매

실험 절차

Add 100 mL of toluene to a nitrogen purged mixture of 2-chloro-4-nitro-pyridine (4.32 g, 27.2 mmol), tert-butyl 4-hydroxypiperidine carboxylate (11.0 g, 54.5 mmol), cesium carbonate (13.3 g, 40.8 mmol), palladium acetate (122 mg, 0.544 mmol) and 2-(di-tert-butylphosphino)-1,1′-binapthyl (271 mg, 0.68 mmol). Stir the resulting mixture overnight at room temperature, then partition between water and ethyl acetate. Extract the aqueous layer with additional ethyl acetate, and dry the combined organic layer over sodium sulfate and concentrate under reduced pressure. Subject residue to silica gel chromatography eluting with a gradient of 0 to 20% ethyl acetate in hexanes to afford 4-(4-nitro-pyridin-2-yloxy)-piperidine-1-carboxylic acid tert-butyl ester as a white waxy solid (5.37 g, 61%; LCMS ES+(m/z) 268 [M-tBu]+).

후처리

  1. custompurged
  2. custompartition between water and ethyl acetate
  3. extractionExtract the aqueous layer with additional ethyl acetate
  4. dry with materialdry the combined organic layer over sodium sulfate
  5. concentrationconcentrate under reduced pressure
  6. washSubject residue to silica gel chromatography eluting with a gradient of 0 to 20% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-aee9de94020a42c59a4939777f686770
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652015B2

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