Ammonium Hydroxide → HCID 178468551, 화합물

HRID 54173

반응식

HRID 54173 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[N:6][C:7]=1[NH2:8].[CH2:19](C(CC)(CC)C([O-])([O-])[O-])[CH3:20].[OH-].[NH4+]>C(O)(=O)C>[CH3:19][C:20]1[N:8]=[C:7]2[NH:6][C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:3]=[C:2]2[N:1]=1

참가 물질

5

반응물 3

HCID 14923Ammonium HydroxideHCID 21847042Diethyl 5,6-diamino-2,3-pyridinedicarboxylateHCID 21875354Triethylorthoaceate

생성물 1

HCID 178468551HCID 178468551, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Diethyl 5,6-diamino-2,3-pyridinedicarboxylate (10.38 g, 0.041 mol) is stirred under an N2 atmosphere in 100 mL glacial acetic acid, to give a clear orange solution. Triethylorthoacetate (TEOA), (0.19 mol) is then added and the mixture is heated to reflux for 15 hours. The cooled solution is poured into ice water and neutralized with ammonium hydroxide. The solution is extracted with ethyl acetate, the combined organic layers washed with brine, dried over Na2SO4, filtered and concentrated to an oil. The oil is taken up in ethyl acetate and the desired product is precipitated by the addition of hexanes in two crops of beige solid, totalling 8.11 g (71.3%), having a melting point of 164°-165° C.

후처리

  1. customto give a clear orange solution
  2. temperaturethe mixture is heated
  3. temperatureto reflux for 15 hours
  4. extractionThe solution is extracted with ethyl acetate
  5. washthe combined organic layers washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated to an oil
  9. customthe desired product is precipitated by the addition of hexanes in two crops of beige solid, totalling 8.11 g (71.3%)

출처 및 근거

ORD 기록
ord-095d813f2b214d1898e6fbd5d65abebe
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622913

연결된 노트

불러오는 중…