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Dimethyl Sulfate → HCID 20291420, 화합물

HRID 1413308
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HRID 1413308 반응식
[CH3:1][C:2]1[N:3]=[C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:5]2[C:10]=1[CH:9]=[N:8][NH:7][C:6]2=[S:11].S(OC)(O[CH3:22])(=O)=O>C(=O)(O)[O-].[Na+]>[CH3:22][N:7]1[C:6](=[S:11])[N:5]2[C:4]([C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)=[N:3][C:2]([CH3:1])=[C:10]2[CH:9]=[N:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6497Dimethyl SulfateHCID 13548752HCID 13548752, 화합물

생성물 1

HCID 20291420HCID 20291420, 화합물수율 7%

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

실험 절차

8-Methyl-6-phenyl-imidazo[1,5-d]-as-triazin-4(3H)-thione (3.76 g, 0.014 mole) is dissolved in aqueous sodium bicarbonate (125 ml. 6.7%). Dimethyl sulfate (1.85 g, 0.0147 mole) is added at room temperature and the reaction mixture stirred overnight (appr. 15-16 hours). The precipitated solid is collected by filtration and washed thoroughly with water. The dried solid (3.84 g) is extracted with benzene. The benzene solution is evaporated to dryness, and the residual red solid obtained is extracted with hexane. Evaporation of the hexane solution yields a tan solid (0.25 g). Recrystallization of this tan solid from methanol yields pale yellow crystals, m.p. 194°-195° C.

후처리

  1. filtrationThe precipitated solid is collected by filtration
  2. washwashed thoroughly with water
  3. extractionThe dried solid (3.84 g) is extracted with benzene
  4. customThe benzene solution is evaporated to dryness
  5. customthe residual red solid obtained
  6. extractionis extracted with hexane
  7. customEvaporation of the hexane solution

출처 및 근거

ORD 기록
ord-daa5c29581764a3a92ed2fd132902862
출처 데이터셋
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE030511

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