Phosphorus sulfide (P2S5) → HCID 178504191, 화합물

HRID 1440995노트

반응식

HRID 1440995 반응식
[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

참가 물질

4

반응물 2

HCID 14817Phosphorus sulfide (P2S5)HCID 178504190HCID 178504190, 화합물

생성물 1

HCID 178504191HCID 178504191, 화합물수율 84.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d36c47f0f804e61997c4f932188b21f
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05502054

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