2,4,6-Trimethylbenzyl chloride → 2-(2,4,6-trimethylphenylmethylthio)pyridine N-oxide

HRID 329139

반응식

HRID 329139 반응식
[SH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:8].[Na].[CH3:10][C:11]1[CH:16]=[C:15]([CH3:17])[C:14]([CH2:18]Cl)=[C:13]([CH3:20])[CH:12]=1>C(O)C>[CH3:20][C:13]1[CH:12]=[C:11]([CH3:10])[CH:16]=[C:15]([CH3:17])[C:14]=1[CH2:18][S:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:8]

참가 물질

5

반응물 3

HCID 741082,4,6-Trimethylbenzyl chlorideHCID 5360545SodiumHCID 178526253HCID 178526253, 화합물

생성물 1

HCID 220547812-(2,4,6-trimethylphenylmethylthio)pyridine N-oxide수율 88.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 17 gms (0.05 mole) 2-mercaptopyridine N-oxide, sodium salt (40% aqueous solution) and 8.5 gms (0.05 mole) α2 chloroisodurene in 50 ml of ethanol is brought to reflux for 15 minutes. The volatiles are removed and the residue extracted with 150 ml of boiling chloroform, filtered and dried over sodium sulfate. Evaporation and trituration of the residue with a few drops of acetone induce crystallization. A yield of 11.5 gms of 2-(2,4,6-trimethylphenylmethylthio)pyridine N-oxide is obtained. Melting point 137° - 138° C. Structure confirmed by IR and NMR.

후처리

  1. temperatureto reflux for 15 minutes
  2. customThe volatiles are removed
  3. extractionthe residue extracted with 150 ml of boiling chloroform
  4. filtrationfiltered
  5. dry with materialdried over sodium sulfate
  6. customEvaporation and trituration of the residue with a few drops of acetone
  7. customcrystallization

출처 및 근거

ORD 기록
ord-aab389400d344cb691183917617e1f32
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04019893

연결된 노트

불러오는 중…