Guanidine Nitrate → HCID 178512737, 화합물

HRID 464703

반응식

HRID 464703 반응식
[N+]([O-])(O)=O.[NH2:5][C:6]([NH2:8])=[NH:7].[H-].[Na+].[H][H].Cl[C:14]1[S:15][C:16]([C:19]2[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=2)=[N:17][N:18]=1>CN(C)C=O.O>[NH:7]([C:14]1[S:15][C:16]([C:19]2[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=2)=[N:17][N:18]=1)[C:6]([NH2:8])=[NH:5]

참가 물질

7

반응물 4

HCID 10481Guanidine NitrateHCID 24758Sodium hydrideHCID 105142772-Chloro-5-(4-nitrophenyl)-1,3,4-thiadiazoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 178512737HCID 178512737, 화합물수율 55%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

24.13 gm of guanidine nitrate were added in small portions over a period of 30 minutes to 6.5 gm of a 50% sodium hydride oil dispersion in 200 ml of dimethylformamide. After the evolution of hydrogen had ceased, a solution 15.8 gm of 2-chloro-5-(4-nitro-phenyl)-1,3,4-thiadiazole in 300 ml of dimethylformamide was added dropwise to the mixture, which was then stirred at room temperature for 2 hours, and then at 90° C. for 30 minutes. After cooling and dilution with water, the precipitate formed thereby was filtered off and dissolved in ethanol. Hydrogen chloride was added to this solution, and the hydrochloride which separated out was filtered off and dissolved in water, and then aqueous solution was made alkaline with 10% sodium hydroxide. The free base was filtered off, washed with water and dried, yielding 9.5 gm of the title compound, m.p. 295°-297° C.

후처리

  1. waitat 90° C. for 30 minutes
  2. temperatureAfter cooling
  3. filtrationthereby was filtered off
  4. dissolutiondissolved in ethanol
  5. additionHydrogen chloride was added to this solution
  6. customthe hydrochloride which separated out
  7. filtrationwas filtered off
  8. dissolutiondissolved in water
  9. filtrationThe free base was filtered off
  10. washwashed with water
  11. customdried

출처 및 근거

ORD 기록
ord-6fcbeec2da374d0289f736b884ea9810
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04548944

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