Heptane → HCID 178524447, 화합물

HRID 478653

반응식

HRID 478653 반응식
C(O[C:4]([C:6]1[CH:7]=[N:8][C:9]2[C:14]([C:15]=1Cl)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])C.[NH:17]([C:19]1[CH:27]=[CH:26][C:22]([C:23]([OH:25])=[O:24])=[CH:21][CH:20]=1)[NH2:18].CCCCCCC>C(O)CCC>[O:5]=[C:4]1[C:6]2=[CH:7][NH:8][C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=3[C:15]2=[N:18][N:17]1[C:19]1[CH:20]=[CH:21][C:22]([C:23]([OH:25])=[O:24])=[CH:26][CH:27]=1

참가 물질

5

반응물 3

HCID 8900HeptaneHCID 120894-Hydrazinobenzoic acidHCID 268963Ethyl 4-Chloroquinoline-3-carboxylate

생성물 1

HCID 178524447HCID 178524447, 화합물수율 8.5%

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
60 °C

실험 절차

A solution of 4-chloro-quinoline-3-carboxylic acid ethyl ester (11.8 mg, 0.5 mmol) and 4-hydrazino-benzoic acid (7.6 mg, 0.5 mmol) in n-butanol (0.5 mL) was stirred at 115° C. over night in a sealed tube. After cooling to 50-70° C., heptane (1.0 mL) was added and the product was allowed to crystallize upon further cooling to room temperature. The solvent was removed and the product was washed with heptane and dried under vacuum to yield 4-(3-oxo-3,5-dihydro-pyrazolo[4,3-c]quinolin-2-yl)-benzoic acid (13 mg). 1H NMR (400 MHz, DMSO-d6) δ 12.9 (1H, s), 8.77 (1H, d), 8.38 (2H, d), 8.25 (1H, d), 8.03 (2H, d), 7.65-7.77 (2H, m), 7.58 (1H, t).

후처리

  1. customto crystallize
  2. temperatureupon further cooling to room temperature
  3. customThe solvent was removed
  4. washthe product was washed with heptane
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-69af56a780f04c518b22da7aedf8bfda
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06642249B2

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