Hydrochloric Acid → HCID 178481844, 화합물

HRID 236228

반응식

HRID 236228 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.C1(N=C=NC2CCCCC2)CCCCC1.C(=O)([O-])[O-].[K+].[K+].[CH3:36][N:37]1[C:41]([OH:42])=[CH:40][CH:39]=[N:38]1.Cl>C(Cl)(Cl)Cl.C(O)(C)(C)C>[Cl:1][C:2]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([C:40]1[CH:39]=[N:38][N:37]([CH3:36])[C:41]=1[OH:42])=[O:6]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 10868DicyclohexylcarbodiimideHCID 11430Potassium CarbonateHCID 7358632-Chloro-4-(methylsulfonyl)benzoic acidHCID 178481816HCID 178481816, 화합물

생성물 1

HCID 178481844HCID 178481844, 화합물수율 53%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6386tert-Butanol용매

실험 절차

2-chloro-4-methanesulfonyl benzoic acid 3.87 g (0.0165 mol) was added to 40 ml of tert.-butanol, and then were added thereto 3.47 g (0.0168 mol) of N,N'-dicyclohexylcarbodiimide and 1.21 g (0.088 mol) of anhydrous potassium carbonate. The resulting mixture was incorporated with 1.65 g (0.0168 mol) of 1-methyl-5-hydroxypyrazole with stirring at room temperature and heated at 60° C. to effect reaction for 5 hours. After completion of the reaction, solvent was distilled away from the reaction mixture under reduced pressure and the resulting residue was washed with chloroform. Thereafter, the residue was incorporated with 30 ml of water and stirred. Insoluble matter was filtered out. The aqueous solution thus obtained was incorporated with conc. hydrochloric acid to adjust the pH thereof to 1 or lower and then with chloroform to effect extraction. An organic layer was separated, dried over anhydrous sodium sulfate, freed of solvent by distillation under reduced pressure, and dried to give 2.75 g of the final product (yield: 53%), m.p. 272°-275° C.

후처리

  1. additionwere added
  2. temperatureheated at 60° C.
  3. customreaction for 5 hours
  4. customAfter completion of the reaction, solvent
  5. distillationwas distilled away from the reaction mixture under reduced pressure
  6. washthe resulting residue was washed with chloroform
  7. stirringstirred
  8. filtrationInsoluble matter was filtered out
  9. customThe aqueous solution thus obtained
  10. extractionextraction
  11. customAn organic layer was separated
  12. dry with materialdried over anhydrous sodium sulfate
  13. distillationfreed of solvent by distillation under reduced pressure
  14. customdried

출처 및 근거

ORD 기록
ord-9de8fd284a304d859132ddddaa3258ef
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04643757

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