Methyl iodide → HCID 68276426, 화합물

HRID 334391노트

반응식

HRID 334391 반응식
[CH3:1]I.[OH:3][C:4]1[C:11]([I:12])=[CH:10][C:7]([C:8]#[N:9])=[C:6]([S:13][CH3:14])[N:5]=1>O1CCOCC1.C(=O)([O-])[O-].[Ag+2]>[I:12][C:11]1[C:4]([O:3][CH3:1])=[N:5][C:6]([S:13][CH3:14])=[C:7]([CH:10]=1)[C:8]#[N:9]

참가 물질

5

반응물 2

HCID 6328Methyl iodideHCID 178503563HCID 178503563, 화합물

생성물 1

HCID 68276426HCID 68276426, 화합물수율 68%

시약·촉매·용매 2

HCID 178418647HCID 178418647, 화합물촉매HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

905 μl (2 eq) of methyl iodide and 2.1 g (1.05 eq) of silver carbonate are added successively to a solution of 2.12 g (7.26 mmol) of 6-hydroxy-5-iodo-2-(methylthio)nicotinonitrile in 20 ml of 1,4-dioxane. The reaction medium is stirred at 60° C. for 5 hours. The solid is filtered and the residue rinsed thoroughly with methanol. The filtrate is evaporated and the residue purified by silica column chromatography (4:6 dichloromethane/cyclohexane as eluent) to yield 1.52 g (68%) of 5-iodo-6-methoxy-2-(methylthio)nicotinonitrile in the form of a white powder.

후처리

  1. filtrationThe solid is filtered
  2. washthe residue rinsed thoroughly with methanol
  3. customThe filtrate is evaporated
  4. customthe residue purified by silica column chromatography (4:6 dichloromethane/cyclohexane as eluent)

출처 및 근거

ORD 기록
ord-a34fad2b8a93477685fc85a3846c464b
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883821B2

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