3-chloromethylpyridine-N-oxide hydrochloride → Pyrimidine, 4-((3-pyridinylmethyl)thio)-, N-oxide

HRID 27883노트

반응식

HRID 27883 반응식
[SH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][N:3]=1.Cl.Cl[CH2:10][C:11]1[CH:12]=[N+:13]([O-:17])[CH:14]=[CH:15][CH:16]=1>C(O)C>[CH:15]1[CH:14]=[N+:13]([O-:17])[CH:12]=[C:11]([CH2:10][S:1][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][N:3]=2)[CH:16]=1

참가 물질

4

반응물 2

HCID 233403793-chloromethylpyridine-N-oxide hydrochlorideHCID 178527731HCID 178527731, 화합물

생성물 1

HCID 3054374Pyrimidine, 4-((3-pyridinylmethyl)thio)-, N-oxide수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

11.2 g (0.1 moles) 4-mercaptopyrimidine is dissolved in 100 ml ethanol containing 10.8 g sodium methoxide. 18 g (0.1 moles) 3-chloromethylpyridine-N-oxide hydrochloride is added; the mixture is heated under reflux for about one hours. The solution is cooled to ambient temperature, the sodium chloride filtered off, and the filtrate evaporated under vacuum to eliminate the solvent. The residue is crystallized from ethyl acetate to give 15.35 g of product (M.P.=105°-108° C.; yield=70%).

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for about one hours
  3. filtrationthe sodium chloride filtered off
  4. customthe filtrate evaporated under vacuum
  5. customThe residue is crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-552ef03457564915a26b6bc959c84103
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04224327

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