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Cesium carbonate → HCID 67273555, 화합물

HRID 1696751
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HRID 1696751 반응식
[CH3:1][S:2][C:3]1[CH:8]=[C:7]([NH2:9])[N:6]=[C:5]([NH2:10])[CH:4]=1.[C:11]([Si:15]([O:18][CH2:19][CH2:20]I)([CH3:17])[CH3:16])([CH3:14])([CH3:13])[CH3:12].C([O-])([O-])=O.[Cs+].[Cs+]>C(#N)C>[C:11]([Si:15]([CH3:17])([CH3:16])[O:18][CH2:19][CH2:20][NH:10][C:5]1[CH:4]=[C:3]([S:2][CH3:1])[CH:8]=[C:7]([NH2:9])[N:6]=1)([CH3:14])([CH3:13])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 11129873tert-Butyl(2-iodoethoxy)dimethylsilaneHCID 672745044-Methylsulfanyl-pyridine-2,6-diamine

생성물 1

HCID 67273555HCID 67273555, 화합물수율 22%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In a glass vessel were mixed together the above prepared 4-methylsulfanyl-pyridine-2,6-diamine (0.350 g, 2.25 mmol), tert-butyl-(2-iodo-ethoxy)-dimethyl-silane (CAS 101166-65-8, 0.700 g, 1.08 eq.), and 1.2 eq. of Cs2CO3 (0.882 g) in 3.5 mL of abs. acetonitrile, and the mixture allowed to react for 2 h at 125° C. in a microwave oven. Cooling, pouring onto crashed ice, twofold extraction with AcOEt, washing with water and brine, drying over sodium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=4/6) afforded 0.155 g of the title compound as light brown oil.

후처리

  1. additionIn a glass vessel were mixed together the
  2. customto react for 2 h at 125° C. in a microwave oven
  3. temperatureCooling
  4. additionpouring
  5. extractionice, twofold extraction with AcOEt
  6. washwashing with water and brine
  7. dry with materialdrying over sodium sulfate, and evaporation of the solvents

출처 및 근거

ORD 기록
ord-c4ae1a5242ec4ad880edf42c07071d8a
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163778B2

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