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Phosphorus sulfide (P2S5) → HCID 86663792, 화합물

HRID 570954
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HRID 570954 반응식
[CH3:1][N:2]1[C:7](=[O:8])[N:6]2[CH:9]=[N:10][C:11]([C:12]([NH:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=O)=[C:5]2[N:4]=[N:3]1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22].C[Si](C)(C)O[Si](C)(C)C>C(Cl)Cl>[CH3:1][N:2]1[C:7](=[O:8])[N:6]2[CH:9]=[N:10][C:11]([C:12](=[S:22])[NH:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[C:5]2[N:4]=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14817Phosphorus sulfide (P2S5)HCID 24764HexamethyldisiloxaneHCID 49869278HCID 49869278, 화합물

생성물 1

HCID 86663792HCID 86663792, 화합물수율 270.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 3-methyl-4-oxo-N-phenyl-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carboxamide (430 mg, 1.59 mmol), phosphorus pentasulfide (212 mg, 0.48 mmol) and hexamethyldisiloxane (680 μL, 3.18 mmol) in DCM (20 mL) was refluxed overnight. The crude product was absorbed on silica and was purified by flash chromatography using a gradient elution of DCM:MeOH (100:0 to 98:2) to give 372 mg of 3-methyl-4-oxo-N-phenyl-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carbothioamide as a 1.5:1 inseparable mixture with the starting material.

후처리

  1. temperaturewas refluxed overnight
  2. customThe crude product was absorbed on silica
  3. customwas purified by flash chromatography
  4. washa gradient elution of DCM:MeOH (100:0 to 98:2)

출처 및 근거

ORD 기록
ord-68770f884d1f4ec9b678718ff4dc0597
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09024018B2

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