Sulfur → 103807-33-6

HRID 2292023ノート

反応式

HRID 2292023 の反応式
[S].[CH3:2][CH:3]1[C:8](=[O:9])[NH:7][C:6]([CH3:10])=[C:5]([CH:11]2[CH:16]=[CH:15][N:14](C(OCC(Cl)(Cl)Cl)=O)[CH:13]=[CH:12]2)[S:4]1>CN(C)C=O.C(Cl)(Cl)Cl>[CH3:2][CH:3]1[C:8](=[O:9])[NH:7][C:6]([CH3:10])=[C:5]([C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)[S:4]1

参加物

5

反応物 2

HCID 5362487SulfurHCID 13805985HCID 13805985、化合物

生成物 1

HCID 11971509103807-33-6収率 52%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
140 °C

実験手順

Sulfur sublimed (0.7 g) was added to a solution of 2,5-dimethyl-6-[1-(2,2,2-trichloroethoxycarbonyl)-1,4-dihydro-4-pyridinyl]-2H-1,4-thiazin-3(4H)-one (1.5 g) in dimethylformamide (20 ml) and the mixture was stirred at 140° C. for 2 hours. Then, the mixture was allowed to cool to ambient temperature and the solvent was removed under reduced pressure. The residue was dissolved in 2N hydrochloric acid and the insoluble matter was removed by filtration. The filtrate was adjusted to pH 7-8 by 2N aqueous sodium hydroxide. The precipitated crude crystals were chromatographed on silica gel (Wakogel C-200) column, using chloroform-methanol (=20:1) as an eluant to give pale yellow crystals. These crude crystals were dissolved in chloroform, were washed with water and were dried over magnesium sulfate. The solvent was removed under reduced pressure to give the titled compound (0.43 g, yield 52%) as white crystals.

後処理

  1. temperatureto cool to ambient temperature
  2. customthe solvent was removed under reduced pressure
  3. dissolutionThe residue was dissolved in 2N hydrochloric acid
  4. customthe insoluble matter was removed by filtration
  5. customThe precipitated crude crystals
  6. customwere chromatographed on silica gel (Wakogel C-200) column
  7. customto give pale yellow crystals
  8. washwere washed with water
  9. dry with materialwere dried over magnesium sulfate
  10. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-a70808b5b08e4502b5eff0b53d09a608
出典データセット
uspto-grants-1989_01
特許番号
US04800201

反応ノート

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