Methanol → 6-Butyl-4-methoxycarbonyl-2-oxo-1,2-dihydropyridine

HRID 234760노트

반응식

HRID 234760 반응식
S(Cl)(Cl)=O.[CH2:5]([C:9]1[NH:10][C:11](=[O:18])[CH:12]=[C:13]([CH:17]=1)[C:14]([OH:16])=[O:15])[CH2:6][CH2:7][CH3:8].[CH3:19]O>>[CH2:5]([C:9]1[NH:10][C:11](=[O:18])[CH:12]=[C:13]([C:14]([O:16][CH3:19])=[O:15])[CH:17]=1)[CH2:6][CH2:7][CH3:8]

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 540903426-Butyl-2-oxo-1,2-dihydro-isonicotinic acid

생성물 1

HCID 152251016-Butyl-4-methoxycarbonyl-2-oxo-1,2-dihydropyridine

실험 절차

12.5 ml (0.17 mol) of thionyl chloride are added dropwise to a suspension of 29.25 g (0.15 mol) of 6-butyl-2-oxo-1,2-dihydro-isonicotinic acid in 200 ml of methanol, while cooling with ice, and the mixture is stirred overnight at room temperature. It is concentrated to dryness and the residue is chromatographed over 450 g of silica gel (230-400 mesh) using methylene chloride→methylene chloride/methanol 10:1. Colourless crystals of melting point 106° C. crystallise from methylene chloride, ether and petroleum ether.

후처리

  1. temperaturewhile cooling with ice
  2. concentrationIt is concentrated to dryness
  3. customthe residue is chromatographed over 450 g of silica gel (230-400 mesh)
  4. customColourless crystals of melting point 106° C. crystallise from methylene chloride, ether and petroleum ether

출처 및 근거

ORD 기록
ord-caceb24978cb4cbc9279bf0a7731c694
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05596006

반응 노트

불러오는 중…