2-Naphthoic acid → HCID 178509287, 화합물

HRID 619340

반응식

HRID 619340 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([OH:13])=O.[NH2:14][C:15]1[N:19]=[C:18]([NH2:20])[NH:17][N:16]=1>O1CCCC1>[NH2:20][C:18]1[N:19]=[C:15]([NH:14][C:11]([C:2]2[CH:3]=[CH:4][C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[CH:1]=2)=[O:13])[NH:16][N:17]=1

참가 물질

4

실험 절차

A mixture of 2-naphthyl carboxylic acid (2.0 g, 11.6 mmol) and N,N'-carbonyldiimidazole (2.07 g, 12.8 mmol) in dry tetrahydrofuran (50 ml) was stirred at reflux temperature for 1 h. To the cooled reaction mixture was added 3,5-diamino-1,2,4-triazole (1.15 g, 11.6 mmol) and the resulting mixture was refluxed for 3 h. The cooled reaction mixture was quenched with water (75 ml) and extracted with diethyl ether (2×75 ml). The combined organic extracts were washed with saturated aqueous sodium chloride (2×50 ml), dried (MgSO4), filtered and evaporated in vacuo. The residue was crystallised from diethyl ether (20 ml), filtered off and washed with diethyl ether (2×10 ml), dried in vacuo afforded 0.95 g (32%) of the title compound as a solid.

후처리

  1. temperatureat reflux temperature for 1 h
  2. customTo the cooled reaction mixture
  3. temperaturethe resulting mixture was refluxed for 3 h
  4. customThe cooled reaction mixture
  5. customwas quenched with water (75 ml)
  6. extractionextracted with diethyl ether (2×75 ml)
  7. washThe combined organic extracts were washed with saturated aqueous sodium chloride (2×50 ml)
  8. dry with materialdried (MgSO4)
  9. filtrationfiltered
  10. customevaporated in vacuo
  11. customThe residue was crystallised from diethyl ether (20 ml)
  12. filtrationfiltered off
  13. washwashed with diethyl ether (2×10 ml)
  14. customdried in vacuo

출처 및 근거

ORD 기록
ord-f4a641cb65cf44cfbed02238990a8b5a
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05958957

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