Hydrochloric Acid → HCID 178515326, 화합물

HRID 37136

반응식

HRID 37136 반응식
[H-].[Na+].[CH:3](OCC)=O.[C:8]1([CH2:14][C:15]([O:17]CC)=O)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[NH2:20][C:21]1[C:25]([C:26]2[CH:31]=[CH:30][C:29]([S:32][C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)=[CH:28][CH:27]=2)=[CH:24][NH:23][N:22]=1.Cl>O.O1CCCC1>[OH:17][C:15]1[N:22]2[N:23]=[CH:24][C:25]([C:26]3[CH:27]=[CH:28][C:29]([S:32][C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)=[CH:30][CH:31]=3)=[C:21]2[N:20]=[CH:3][C:14]=1[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 7590Ethyl phenylacetateHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 178509258HCID 178509258, 화합물

생성물 1

HCID 178515326HCID 178515326, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To tetrahydrofuran suspension of 480 mg of 60% sodium hydride, 2 ml of ethyl formate and 1.64 g of ethyl phenylacetate were added in nitrogen atmosphere, and stirred for 19 hours at room temperature. Adding 1.0 g of 3-amino-4-(4-phenylthiophenyl)pyrazole, the mixture was stirred for 4 hours under reflux. After allowing to cool, water and 10% hydrochloric acid was added. The solution obtained was extracted with ethyl acetate. After washing with water, the organic layer was dried over anhydrous sodium sulfate, and the solvent is distilled off. The residue was dissolved in 5 ml of acetic acid, and the mixture was heated and stirred for 2 to 20 hours at 120° C. After allowing to cool, ethyl acetate was added, and the precipitate was filtered. The filtrate was washed with ethyl acetate and ether and dried, and the title compound was obtained (270 mg, 18%).

후처리

  1. additionwere added in nitrogen atmosphere
  2. stirringthe mixture was stirred for 4 hours
  3. temperatureunder reflux
  4. temperatureto cool
  5. customThe solution obtained
  6. extractionwas extracted with ethyl acetate
  7. washAfter washing with water
  8. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  9. distillationthe solvent is distilled off
  10. dissolutionThe residue was dissolved in 5 ml of acetic acid
  11. temperaturethe mixture was heated
  12. stirringstirred for 2 to 20 hours at 120° C
  13. temperatureto cool
  14. additionethyl acetate was added
  15. filtrationthe precipitate was filtered
  16. washThe filtrate was washed with ethyl acetate and ether
  17. customdried

출처 및 근거

ORD 기록
ord-1eeb9566299843d08dca2af3b8d922f8
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420128

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