Methyl iodide → 1-Methyl-3-iodo-4-methoxypyridin-2-one

HRID 19659ノート

反応式

HRID 19659 の反応式
O[C:2]1[C:7]([I:8])=[C:6]([OH:9])[CH:5]=[CH:4][N:3]=1.[C:10]([O-:13])([O-])=O.[Cs+].[Cs+].[CH3:16]I>CN(C=O)C>[CH3:2][N:3]1[CH:4]=[CH:5][C:6]([O:9][CH3:16])=[C:7]([I:8])[C:10]1=[O:13]

参加物

5

反応物 3

HCID 6328Methyl iodide2 回HCID 10796Cesium carbonateHCID 178516519HCID 178516519、化合物

生成物 1

HCID 226606561-Methyl-3-iodo-4-methoxypyridin-2-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
40 °C

実験手順

A mixture of 2,4-dihydroxy-3-iodopyridine (1.0 eq), Cs2CO3 (2.0 eq), MeI (10.0 eq) and anhydrous DMF was stirred at 40° C. for 72 h, and then the DMF and remaining MeI were evaporated. The residue was treated with aqueous NaS2O3, and the mixture was extracted five times with CH2Cl2. The CH2Cl2 extracts were treated with MgSO4, filtered, and evaporated. The residue was recrystallized from hexanes/CH2Cl2 to give 1-methyl-3-iodo-4-methoxypyridin-2-one.

後処理

  1. customwere evaporated
  2. additionThe residue was treated with aqueous NaS2O3
  3. extractionthe mixture was extracted five times with CH2Cl2
  4. additionThe CH2Cl2 extracts were treated with MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was recrystallized from hexanes/CH2Cl2

出典と根拠

ORDレコード
ord-5a98d1f395ff43d281d83129ab2b6e90
出典データセット
uspto-grants-2010_06
特許番号
US07745454B2

反応ノート

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