Triethylamine → HCID 86650597, 화합물

HRID 1257409

반응식

HRID 1257409 반응식
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[C:11]([CH2:14][NH:15][NH:16][C:17](OC(C)(C)C)=O)[S:12][CH:13]=2)[CH:6]=[CH:7][CH:8]=1.CN(C=[C:30]([C:36](=O)[C:37]([F:40])([F:39])[F:38])[C:31]([O:33][CH2:34][CH3:35])=[O:32])C.C(N(CC)CC)C>C(O)C>[F:38][C:37]([F:39])([F:40])[C:36]1[N:15]([CH2:14][C:11]2[S:12][CH:13]=[C:9]([C:5]3[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:24])[F:25])[CH:4]=3)[N:10]=2)[N:16]=[CH:17][C:30]=1[C:31]([O:33][CH2:34][CH3:35])=[O:32]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 53979199Butanoic acid, 2-[(dimethylamino)methylene]-4,4,4-trifluoro-3-oxo-, ethyl esterHCID 66939173Tert-butyl 2-({4-[3-(trifluoromethyl)phenyl]-1,3-thiazol-2-yl}methyl)hydrazinecarboxylate

생성물 1

HCID 86650597HCID 86650597, 화합물수율 69.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of the compound (0.16 g) obtained in Example 103c, ethyl 2-[(dimethylamino)methylidene]-4,4,4-trifluoro-3-oxobutanoate (0.10 g), triethylamine (0.21 mL) and ethanol (4 mL) was heated under reflux for 16 hr. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate and saturated brine. The ethyl acetate layer was separated, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (0.13 g) as a colorless oil.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. customThe ethyl acetate layer was separated
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-f032328639a14c0ea6a73d18ced22239
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461348B2

연결된 노트

불러오는 중…