Phosphorus sulfide (P2S5) → HCID 178504191、化合物

HRID 1440995ノート

反応式

HRID 1440995 の反応式
[NH2:1][C:2]1[N:3]=[N:4][C:5]([CH2:9][CH2:10][CH2:11][Si:12]([CH3:20])([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:13])=[C:6](O)[N:7]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>N1C=CC=CC=1>[NH2:1][C:2]1[N:3]=[N:4][C:5]([CH2:9][CH2:10][CH2:11][Si:12]([CH3:20])([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:13])=[C:6]([SH:22])[N:7]=1

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 178504190HCID 178504190、化合物

生成物 1

HCID 178504191HCID 178504191、化合物収率 84.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In a flask were placed 2.90 g (0.0105 mole) of 3-amino-5-hydroxy-6-(4-methyl-4-phenyl-4-silapentyl)-1,2,4-triazine, 8.94 g (0.0201 mole) of phosphorus pentasulfide, and 40 mL of pyridine. This mixture was heated at reflux under a nitrogen atmosphere for one hour. The reaction mixture was concentrated under reduced pressure to a volume of approximately 25 mL and then mixed with 150 mL of ice water. The resulting mixture was warmed on a steam bath for 4 hours after which it was cooled to ambient temperature. An orange solid was collected from this mixture by filtration and was stirred with 60 mL of methanol. Filtration of this mixture yielded 2.70 g of 3-amino-5-mercapto-6-(4-methyl-4-phenyl-4-silapentyl)-1,2,4-triazine, m.p. 255°-257° C. (decomposition). The NMR and IR spectra were consistent with the proposed structure.

後処理

  1. customIn a flask were placed
  2. temperatureThis mixture was heated
  3. temperatureat reflux under a nitrogen atmosphere for one hour
  4. concentrationThe reaction mixture was concentrated under reduced pressure to a volume of approximately 25 mL
  5. additionmixed with 150 mL of ice water
  6. temperatureThe resulting mixture was warmed on a steam bath for 4 hours after which it
  7. filtrationAn orange solid was collected from this mixture by filtration
  8. filtrationFiltration of this mixture

出典と根拠

ORDレコード
ord-6d36c47f0f804e61997c4f932188b21f
出典データセット
uspto-grants-1996_03
特許番号
US05502054

反応ノート

読み込み中…