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

HRID 1657331
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HRID 1657331 반응식
[SH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:8].[Na].Cl[CH2:11][C:12]1[CH:20]=[C:18]([CH3:19])[CH:17]=[C:15]([CH3:16])[C:13]=1[CH3:14]>C(O)C>[CH3:11][C:12]1[CH:20]=[C:18]([CH3:19])[CH:17]=[C:15]([CH3:16])[C:13]=1[CH2:14][S:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5360545SodiumHCID 223236781-(Chloromethyl)-2,3,5-trimethylbenzeneHCID 178526253HCID 178526253, 화합물

생성물 1

HCID 220547812-(2,4,6-trimethylphenylmethylthio)pyridine N-oxide

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) α 2 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 induced 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-7fa0ddf893044b9ea3298008acafb611
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03960542

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