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

HRID 27883ノート

反応式

HRID 27883 の反応式
[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

参加物

4

反応物 2

HCID 233403793-chloromethylpyridine-N-oxide hydrochlorideHCID 178527731HCID 178527731、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-552ef03457564915a26b6bc959c84103
出典データセット
uspto-grants-1980_09
特許番号
US04224327

反応ノート

読み込み中…