Iodine → HCID 178503563, 화합물

HRID 1048754노트

반응식

HRID 1048754 반응식
[I:1]I.[OH:3][C:4]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[C:6]([S:12][CH3:13])[N:5]=1>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[OH:3][C:4]1[C:11]([I:1])=[CH:10][C:7]([C:8]#[N:9])=[C:6]([S:12][CH3:13])[N:5]=1

참가 물질

5

반응물 2

HCID 807IodineHCID 178503531HCID 178503531, 화합물

생성물 1

HCID 178503563HCID 178503563, 화합물수율 90.7%

시약·촉매·용매 2

HCID 178418844HCID 178418844, 화합물촉매HCID 702Ethanol용매

실험 절차

6 g (1.6 eq) of silver sulfate and 4.58 g (1.5 eq) of iodine are added successively to a solution of 2 g (12 mmol) of 6-hydroxy-2-(methylthio)nicotinonitrile in 200 ml of ethanol. The reaction medium is stirred at room temperature for 2 hours. The solid is filtered and the residue rinsed thoroughly with methanol. The filtrate is evaporated and then taken up in ethyl acetate. The organic phase is washed with water three times, dried on magnesium sulfate and evaporated to yield 3.18 g (90%) of 6-hydroxy-5-iodo-2-(methylthio)nicotinonitrile in the form of a yellow powder.

후처리

  1. filtrationThe solid is filtered
  2. washthe residue rinsed thoroughly with methanol
  3. customThe filtrate is evaporated
  4. washThe organic phase is washed with water three times
  5. customdried on magnesium sulfate
  6. customevaporated

출처 및 근거

ORD 기록
ord-57539934857c4e78a45be677c930a753
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09381195B2

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