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Hydrochloric Acid → HCID 10899987, 화합물

HRID 2210984
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HRID 2210984 반응식
[CH2:1]([O:3][C:4]1[N:9]2[C:10](=[S:13])[NH:11][N:12]=[C:8]2[CH:7]=[C:6]([F:14])[N:5]=1)[CH3:2].[O-]CC.[Na+].Cl>C(O)C>[CH2:1]([O:3][C:4]1[N:12]2[NH:11][C:10](=[S:13])[N:9]=[C:8]2[CH:7]=[C:6]([F:14])[N:5]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 118060545-ethoxy-7-fluoro-2H-(1,2,4)triazolo(4,3-c)pyrimidine-3-thione

생성물 1

HCID 10899987HCID 10899987, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A mixture of 5.8 g (26 mmol) of 5-ethoxy-7-fluoro-1,2,4-triazolo[4,3-c]pyrimidine-3(2H)-thione in 50 mL of absolute ethanol was prepared and to this was added at 0° C. with vigorous stirring and cooling 12.2 mL (33 mmol) of 21 weight percent sodium ethoxide in ethanol. A mildly exothermic reaction took place and the mixture changed from a suspension to a plum colored solution. The mixture was stirred at below 10° C. for 2.25 hours to complete the reaction. It was then acidified with 25 mL of 1.25N hydrochloric acid, stirred at -10° C. for 30 min, and filtered to recover the precipitate that formed. The precipitate was washed with 10 mL of cold water and dried to obtain 3.3 g (60 percent of theory) of the title compound of 98 percent purity. A second crop amounting to 1.7 g of 60 percent purity material (19 percent of theory) was obtained from the filtrate. The title compound melts at 83.5° C. to 86.5° C. and is a white solid.

후처리

  1. customwas prepared
  2. additionto this was added at 0° C.
  3. customA mildly exothermic reaction
  4. stirringThe mixture was stirred at below 10° C. for 2.25 hours
  5. customthe reaction
  6. stirringstirred at -10° C. for 30 min
  7. filtrationfiltered
  8. customto recover the precipitate
  9. customthat formed
  10. washThe precipitate was washed with 10 mL of cold water
  11. customdried

출처 및 근거

ORD 기록
ord-b0da34e3449b4812909f77013bf217b9
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05461153

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