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

HRID 19659노트

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HRID 19659 반응식
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]

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 10796Cesium carbonateHCID 178516519HCID 178516519, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

반응 조건

온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5a98d1f395ff43d281d83129ab2b6e90
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745454B2

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