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Sodium hydride → 4-(Dimethylamino)pyridine

HRID 1653931
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HRID 1653931 반응식
[C:1](C1CCC(CCC2C=CC(CCC)=CC=2)(C(OC(C)(C)C)=O)C=1)(OCC)=O.[H-].[Na+].C(C(CCC1C=CC(CCC)=CC=1)C(OC(C)(C)C)=O)=O.F[B-](F)(F)F.C(C1([P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)CC1)(OCC)=O.[CH3:84][N:85]1[CH2:90][CH2:89][CH2:88][N:87]([CH3:91])[C:86]1=O>>[CH3:86][N:87]([CH3:91])[C:88]1[CH:89]=[CH:90][N:85]=[CH:84][CH:1]=1
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참가 물질

6

반응물 5

HCID 24758Sodium hydrideHCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-HCID 11016017(1-(Ethoxycarbonyl)cyclopropyl)triphenylphosphonium tetrafluoroborateHCID 15295658HCID 15295658, 화합물HCID 15295659HCID 15295659, 화합물

생성물 1

HCID 142844-(Dimethylamino)pyridine

실험 절차

##STR28## tert-Butyl 3-carbethoxy-1-(2-(4-propylphenyl)ethyl)-2-cyclopentene-1-carboxylate. Sodium hydride (16 mg of 60% oil dispersion, 0.40 mmol) was added to a solution of 102 mg (0.35 mmol) of tert-butyl 2-formyl-4-(4-propylphenyl)butanoate in 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (1.5 mL). After 20 min., 1-carboethoxycyclopropyl triphenylphosphonium tetrafluoroborate (193 mg, 0.42 mmol) was added to the pale yellow solution and stirring was continued overnight at room temperature. The solution was then partitioned between hexane (25 mL) and 2N aq. HCl (25 mL). The organic layer was washed with water (15 mL) and saturated aq. NaCl (15 mL), dried (Na2SO4), decanted, and evaporated. The residue was purified by flash column chromatography on silica gel (8 g), eluting with 100 mL of 5% EtOAc/hexane, to give the title compound as 52 mg (38% yield) of colorless oil.

후처리

  1. waitwas continued overnight at room temperature
  2. customThe solution was then partitioned between hexane (25 mL) and 2N aq. HCl (25 mL)
  3. washThe organic layer was washed with water (15 mL) and saturated aq. NaCl (15 mL)
  4. dry with materialdried (Na2SO4)
  5. customdecanted
  6. customevaporated
  7. customThe residue was purified by flash column chromatography on silica gel (8 g)
  8. washeluting with 100 mL of 5% EtOAc/hexane

출처 및 근거

ORD 기록
ord-01b38a5c97fb4ba88abf4fc3b0be34ca
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05403952

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