2,3-Dichloro-5-(chloromethyl)pyridine → 2,3-Dichloro-5-(methoxymethyl)pyridine

HRID 582812

반응식

HRID 582812 반응식
[CH3:1][O-:2].[Na+].[Cl:4][C:5]1[C:10]([Cl:11])=[CH:9][C:8]([CH2:12]Cl)=[CH:7][N:6]=1>CO>[Cl:4][C:5]1[C:10]([Cl:11])=[CH:9][C:8]([CH2:12][O:2][CH3:1])=[CH:7][N:6]=1

참가 물질

4

반응물 2

HCID 101765362,3-Dichloro-5-(chloromethyl)pyridineHCID 10942334Sodium Methoxide

생성물 1

HCID 111379602,3-Dichloro-5-(methoxymethyl)pyridine

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

Under argon and at room temperature, 4.14 g (23 mmol) of sodium methoxide (30 percent strength solution in methanol) was added dropwise within 5 minutes to a solution of 4.11 g (20.9 mmol) of 2,3-dichloro-5-(chloromethyl)-pyridine [prepared from 2,3-dichloro-5-(hydroxymethyl)-pyridine by reaction with thionyl chloride] in 40 ml of methanol. The reaction mixture was subsequently heated to 60° C. for 3 hours. After the reaction had ended, the solvent was distilled off and the residue was admixed with 100 ml of water and extracted with dichloromethane (3×75 ml). The organic phase was dried over magnesium sulfate and evaporated. The yield of the product was 4.06 g (90.4 percent) of a yellow oil, purity (GC) 90.8 percent.

후처리

  1. distillationthe solvent was distilled off
  2. extractionextracted with dichloromethane (3×75 ml)
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. customevaporated

출처 및 근거

ORD 기록
ord-417f070d4f034bef938334c2140ee6ab
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925765

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