Diiodomethane → 2-Iodo-4-methyl-5-nitropyridine

반응식

N[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.S([O-])(OCCC(C)C)=O.[I:21]CI>>[I:21][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1

참가 물질

반응물 3

HCID 6346Diiodomethane

HCID 2431652-Amino-4-methyl-5-nitropyridine

HCID 22742080Isopentyl sulfite

생성물 1

HCID 230701672-Iodo-4-methyl-5-nitropyridine

반응 조건

온도: 80 °C

실험 절차

To a solution of 1.0 g of 2-amino-4-methyl-5-nitropyridine in 10 mL of diiodomethane was added 1.8 mL of isopentyl sulfite at room temperature, stirred at this temperature for 30 minutes, and after raising the temperature to 80° C., the solution was stirred for 2 hours. The diiodomethane was evaporated, and the crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:20), to afford 897 mg of the title compound as colorless crystals.

후처리

stirringthe solution was stirred for 2 hours
customThe diiodomethane was evaporated
customthe crude product was purified
customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:20)

출처 및 근거

ORD 기록: ord-4591426222324116a52532a1d4076497
출처 데이터셋: uspto-grants-2008_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07429609B2

반응 노트

불러오는 중…