Toluene → S-[(6-Chloro-5-oxo-5H-thiazolo[3,2-a]pyrimidin-7-yl)methyl] O,O-dimethyl phosphorodithioate

HRID 1075294ノート

反応式

HRID 1075294 の反応式
[Cl:1][C:2]1[C:7](=[O:8])[N:6]2[CH:9]=[CH:10][S:11][C:5]2=[N:4][C:3]=1[CH2:12]Cl.C1(C)C=CC=CC=1.[P:21]([S-:27])(=[S:26])([O:24][CH3:25])[O:22][CH3:23].[NH4+]>CO>[P:21]([S:27][CH2:12][C:3]1[N:4]=[C:5]2[S:11][CH:10]=[CH:9][N:6]2[C:7](=[O:8])[C:2]=1[Cl:1])(=[S:26])([O:24][CH3:25])[O:22][CH3:23]

参加物

5

反応物 3

HCID 1140TolueneHCID 6451175Ammonium O,O-dimethyl dithiophosphateHCID 132329226-Chloro-7-(chloromethyl)-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one

生成物 1

HCID 13232940S-[(6-Chloro-5-oxo-5H-thiazolo[3,2-a]pyrimidin-7-yl)methyl] O,O-dimethyl phosphorodithioate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The compound of EXAMPLE 2 (7 g) and 100 ml of toluene was stirred and heated to 70°. To this mixture was added, dropwise, a solution of 14 g ammonium dimethyl phosphorodithioate in 200 ml methanol. The resulting mixture was kept at 70° for 6 hours, then the methanol was distilled off. Toluene (400 ml) was added, and the mixture was washed with water, separated, dried and evaporated under reduced pressure. The solid which remained was washed with toluene and filtered. The solid, m.p. 125°-130°, weighed 2.5 g.

後処理

  1. temperatureheated to 70°
  2. additionTo this mixture was added
  3. distillationthe methanol was distilled off
  4. additionToluene (400 ml) was added
  5. washthe mixture was washed with water
  6. customseparated
  7. customdried
  8. customevaporated under reduced pressure
  9. washThe solid which remained was washed with toluene
  10. filtrationfiltered

出典と根拠

ORDレコード
ord-40ccea17e8c74c6ab6bb42fa09a6de52
出典データセット
uspto-grants-1983_07
特許番号
US04395551

反応ノート

読み込み中…