2-Chloro-4-cyanopyridine → 2-Methoxyisonicotinonitrile

HRID 224870

반응식

HRID 224870 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][O-:11].[Na+]>CO.O1CCOCC1.CO>[CH3:10][O:11][C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1

참가 물질

5

반응물 2

HCID 5686382-Chloro-4-cyanopyridineHCID 10942334Sodium Methoxide

생성물 1

HCID 72048872-Methoxyisonicotinonitrile수율 110.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 21966525Dioxane Methanol용매

실험 절차

2-Chloro-4-cyanopyridine (115.53 g) in methanol/dioxan (1:1, 850 ml) was added to a solution of sodium methoxide (prepared from 20.8 g sodium) in methanol (285 ml) and the mixture was boiled under reflux for 2.5 hours and was allowed to cool. The mixture was filtered and the volume of the filtrate was reduced by evaporation to 200 ml and water (400 ml) was added. The solid which precipitated out was filtered off to give 2-methoxy-4-cyanopyridine (57.2 g, 51%) m.p. 93°-95.5°.

후처리

  1. temperatureunder reflux for 2.5 hours
  2. temperatureto cool
  3. filtrationThe mixture was filtered
  4. customthe volume of the filtrate was reduced by evaporation to 200 ml and water (400 ml)
  5. additionwas added
  6. customThe solid which precipitated out
  7. filtrationwas filtered off

출처 및 근거

ORD 기록
ord-fc4a7db47d314a38aaadf270ddc84200
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234588

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