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Acetic Acid → 5-Fluoromethyl-7-methoxy-N-(2,6-dichlorophenyl)-1,2,4-triazolo[1,5-a]pyrimidine-2-sulfonamide

HRID 1111271
ノート
印刷プレビュー

反応式

HRID 1111271 の反応式
C[Si](C)(C)[NH:3][C:4]1[C:9]([Cl:10])=[CH:8][CH:7]=[CH:6][C:5]=1[Cl:11].[F:14][CH2:15][C:16]1[CH:21]=[C:20](Cl)[N:19]2[N:23]=[C:24]([S:26](Cl)(=[O:28])=[O:27])[N:25]=[C:18]2[N:17]=1.CS(C)=O.[C:34](O)(=[O:36])C>C(#N)C.C(Cl)Cl>[F:14][CH2:15][C:16]1[CH:21]=[C:20]([O:36][CH3:34])[N:19]2[N:23]=[C:24]([S:26]([NH:3][C:4]3[C:9]([Cl:10])=[CH:8][CH:7]=[CH:6][C:5]=3[Cl:11])(=[O:28])=[O:27])[N:25]=[C:18]2[N:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 679Dimethyl SulfoxideHCID 143626792,6-Dichloro-N-trimethylsilylanilineHCID 146234725-Fluoromethyl-7-chloro-1,2,4-triazolo[1,5-a]pyrimidine-2-sulfonyl chloride

生成物 1

HCID 146234745-Fluoromethyl-7-methoxy-N-(2,6-dichlorophenyl)-1,2,4-triazolo[1,5-a]pyrimidine-2-sulfonamide

試薬・触媒・溶媒 2

HCID 6342
Acetonitrile
溶媒
HCID 6344Dichloromethane溶媒

実験手順

A solution containing 3.08 g (13.1 mmol) of N-trimethylsilyl-2,6-dichloroaniline and 1.50 g (5.26 mmol) of 5-fluoromethyl-7-chloro-1,2,4-triazolo[1,5-a]pyrimidine-2-sulfonyl chloride in 15 ml of dry acetonitrile was prepared and 0.075 ml (1.05 mmol) of dimethyl sulfoxide was added with stirring at ambient temperature. The mixture was allowed to react over 4 days and the resulting brown solution was then diluted with 150 ml of methylene chloride, washed with water, and dried over magnesium sulfate. The solvent was removed by evaporation under reduced pressure and replaced with hexane to obtain, after collection of the solids and drying, 1.80 g (84 percent of theory) of the 7-chloro analog of the title compound in about 80 percent purity. This was dissolved in 25 ml of dry methanol, the solution cooled to 0°-5° C. and a mixture of 1.70 g (7.89 mmol) of 25 weight percent sodium methoxide in methanol and 5 ml of methanol was added dropwise with stirring over a 10 min. period. The mixture was allowed to react for 10 min. and then about 1 ml of acetic acid was added. The solid that formed was collected, washed with methanol and with water, and dried to obtain 1.15 g (54 percent of theory) of the title compound as a light brown solid. This was extracted by stirring in boiling methanol, cooling, collecting the solids, and drying to obtain 1.09 g of product melting at 189°-191° C. The proton and fluorine nmr spectra were compatible with the assigned structure.

後処理

  1. customwas prepared
  2. customto react over 4 days
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed by evaporation under reduced pressure
  6. customto obtain
  7. customafter collection of the solids
  8. customdrying
  9. dissolutionThis was dissolved in 25 ml of dry methanol
  10. temperaturethe solution cooled to 0°-5° C.
  11. additiona mixture of 1.70 g (7.89 mmol) of 25 weight percent sodium methoxide in methanol and 5 ml of methanol
  12. additionwas added dropwise
  13. stirringwith stirring over a 10 min. period
  14. customto react for 10 min.
  15. customThe solid that formed
  16. customwas collected
  17. washwashed with methanol and with water
  18. customdried

出典と根拠

ORDレコード
ord-484bfe5c6e69428f8fad0145593a2bfd
出典データセット
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04979981

反応ノート

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