Iodine → HCID 178503563、化合物

HRID 1487361ノート

反応式

HRID 1487361 の反応式
[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

参加物

5

反応物 2

HCID 807IodineHCID 178503531HCID 178503531、化合物

生成物 1

HCID 178503563HCID 178503563、化合物収率 90.7%

試薬・触媒・溶媒 2

HCID 178418844HCID 178418844、化合物触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f10d0fa607e1427caddceec7135719a9
出典データセット
uspto-grants-2016_08
特許番号
US09428510B2

反応ノート

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