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tert-Butanol → Methyl-3-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)benzoate

HRID 338671
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HRID 338671 반응식
C(=O)([O-])[O-].[Cs+].[Cs+].CC(O)(C)C.[CH2:12]1[O:21][C:15]2([CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[O:14][CH2:13]1.[CH3:22][O:23][C:24](=[O:32])[C:25]1[CH:30]=[CH:29][CH:28]=[C:27](Br)[CH:26]=1>C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C>[CH3:22][O:23][C:24](=[O:32])[C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([N:18]2[CH2:19][CH2:20][C:15]3([O:21][CH2:12][CH2:13][O:14]3)[CH2:16][CH2:17]2)[CH:26]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6386tert-Butanol2회HCID 10796Cesium carbonateHCID 12070Methyl 3-bromobenzoateHCID 674351,4-Dioxa-8-azaspiro(4.5)decane

생성물 1

HCID 60059302Methyl-3-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)benzoate수율 97.1%

시약·촉매·용매 3

HCID 167845
palladium(II) acetate
촉매
HCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl촉매
HCID 1140Toluene용매2회

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온도
120 °C

실험 절차

Procedure adopted from Tetrahedron Lett., 2007, 48, 2519. A thick-walled glass reaction vessel was charged with palladium(II)acetate (235 mg, 1.05 mmol), X-Phos (500 mg, 1.05 mmol, 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl), cesium carbonate (6.82 g, 20.95 mmol) and 5:1 (v/v) toluene:t-BuOH (20 mL). The stirred contents were purged with nitrogen and a solution of 4-piperidone ethylene ketal (2.70 mL, 20.95 mmol) and methyl-3-bromobenzoate (4.95 g, 23.02 mmol) in 5:1 (v/v) toluene:t-BuOH (100 mL) was added. After stirring for 2 minutes, the vessel was sealed and the reaction mixture was heated at 120° C. for 16 hours. Upon cooling to room temperature, the reaction mixture was filtered through celite and the filtrate was concentrated. Elution through a flash column (silica gel 60, 230-400 mesh, 7:3 hexanes:EtOAc) followed by concentration gave the title compound as an oil (5.64 g, 97%).

후처리

  1. customA thick-walled glass reaction vessel
  2. customThe stirred contents were purged with nitrogen
  3. customthe vessel was sealed
  4. temperatureUpon cooling to room temperature
  5. filtrationthe reaction mixture was filtered through celite
  6. concentrationthe filtrate was concentrated
  7. washElution through a flash column (silica gel 60, 230-400 mesh, 7:3 hexanes:EtOAc)
  8. concentrationfollowed by concentration

출처 및 근거

ORD 기록
ord-761c5256799d4ab7bd44e14652109788
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889870B2

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