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Tributyltin Chloride → (3-Tributylstannyl-pyridin-4-yl)-carbamic acid tert-butyl ester

HRID 8734
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HRID 8734 반응식
[C:1]([O:5][C:6](=[O:14])[NH:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].C([Li])(C)(C)C.[CH2:20]([Sn:24](Cl)([CH2:29][CH2:30][CH2:31][CH3:32])[CH2:25][CH2:26][CH2:27][CH3:28])[CH2:21][CH2:22][CH3:23].[Cl-].[NH4+]>C1COCC1>[C:1]([O:5][C:6](=[O:14])[NH:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][C:9]=1[Sn:24]([CH2:25][CH2:26][CH2:27][CH3:28])([CH2:29][CH2:30][CH2:31][CH3:32])[CH2:20][CH2:21][CH2:22][CH3:23])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 4

HCID 15096Tributyltin ChlorideHCID 25517Ammonium ChlorideHCID 99902104-(Boc-amino)pyridineHCID 178418306HCID 178418306, 화합물

생성물 1

HCID 69595531(3-Tributylstannyl-pyridin-4-yl)-carbamic acid tert-butyl ester수율 49%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
-78 °C

실험 절차

Pyridin-4-yl-carbamic acid tert-butyl ester (1.74 g, 8.95 mmol) (prepared as described in Venuti et al, J. Med. Chem. 1988, 31(11), 2136–45) dissolved in THF (150 mL) was cooled to −78° C. and a solution of 1.7M tert-butyllithium in hexanes (11.6 mL, 19.70 mmol) was added dropwise. After the addition, the stirring was continued for 1 h to −78° C. and the solution was then allowed to warm to −20° C. and stirred for an additional 3 h. The reaction was cooled again to −78° C. and tributyltin chloride (2.91 mL, 10.74 mmol) was added dropwise and the reaction was allowed to reach room temperature overnight. A saturated ammonium chloride solution was added and the product extracted with dichloromethane. The combined organics were dried over magnesium sulfate, the solvent was evaporated and residue purified by flash chromatography eluting with 20% ethyl acetate in hexanes to yield 2.12 g of (3-tributylstannyl-pyridin-4-yl)-carbamic acid tert-butyl ester.

후처리

  1. additionAfter the addition
  2. temperatureto warm to −20° C.
  3. temperatureThe reaction was cooled again to −78° C.
  4. waitto reach room temperature overnight
  5. extractionthe product extracted with dichloromethane
  6. dry with materialThe combined organics were dried over magnesium sulfate
  7. customthe solvent was evaporated
  8. customresidue purified by flash chromatography
  9. washeluting with 20% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-1fa2eca5f3db433194f7dea595645644
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091200B2

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