Water → 2-Ethoxy-4-iodo-3,5-dimethylpyridine

HRID 1043926노트

반응식

HRID 1043926 반응식
[O-:1][CH2:2][CH3:3].[Na+].F[C:6]1[C:11]([CH3:12])=[C:10]([I:13])[C:9]([CH3:14])=[CH:8][N:7]=1.CC(OC)(C)C.O>C(O)C.C1COCC1>[CH2:2]([O:1][C:6]1[C:11]([CH3:12])=[C:10]([I:13])[C:9]([CH3:14])=[CH:8][N:7]=1)[CH3:3]

참가 물질

7

반응물 4

HCID 962WaterHCID 15413tert-Butyl methyl etherHCID 2723922Sodium ethoxideHCID 735548982-Fluoro-4-iodo-3,5-dimethylpyridine

생성물 1

HCID 866863502-Ethoxy-4-iodo-3,5-dimethylpyridine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A 20% solution of sodium ethoxide in ethanol (123 mL) was added to a solution of 2-fluoro-4-iodo-3,5-dimethylpyridine obtained in Preparation Example 29(2) (400 mg) in THF (5 mL), and the mixed solution was stirred at room temperature overnight. The reaction mixture was cooled at 0° C., and MTBE (20 mL) and water (20 mL) were then added. The organic layer was separated. The organic layer was washed with brine. The combined aqueous layers were extracted with MTBE. The combined organic layers were dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to give the title compound (423.8 mg).

후처리

  1. temperatureThe reaction mixture was cooled at 0° C.
  2. customThe organic layer was separated
  3. washThe organic layer was washed with brine
  4. extractionThe combined aqueous layers were extracted with MTBE
  5. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-670cee03402942f08d5cfc92d6af8fae
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563565B2

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