Acetic Acid → HCID 14855575, 화합물

HRID 477388노트

반응식

HRID 477388 반응식
[CH2:1]([NH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[CH3:2].[F:10][C:11]([F:23])([F:22])[C:12]1[CH:16]=[C:15]([O:17][CH2:18][C:19](O)=[O:20])[O:14][N:13]=1.C1(N=C=NC2CCCCC2)CCCCC1.C(O)(=O)C>C1COCC1>[CH2:1]([N:3]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[C:19](=[O:20])[CH2:18][O:17][C:15]1[O:14][N:13]=[C:12]([C:11]([F:23])([F:10])[F:22])[CH:16]=1)[CH3:2]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 7670N-EthylanilineHCID 10868DicyclohexylcarbodiimideHCID 14855464HCID 14855464, 화합물

생성물 1

HCID 14855575HCID 14855575, 화합물수율 85.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1.30 ml (2.37 mmole) of N-ethylaniline and 0.50 g (2.37 mmole) of 2-(3-trifluoromethyl-5-isoxazolyloxy)acetic acid were dissolved in 2.4 ml of dry THF and to the solution was added 0.60 g (2.61 mmole) of dicyclohexylcarbodiimide. After being stirred at room temperature for one hour, the reaction mixture was allowed to stand overnight at room temperature. After the addition of glacial acetic acid (0.2 ml), the mixture was stirred at room temperature for 30 minutes and the precipitated crystals were filtered off. The filtrate was evaporated under reduced pressure and the residue was purified by chromatography on silica gel to give 638 mg of the titled compound as a pale red viscous liquid, yield 85.7%.

후처리

  1. waitto stand overnight at room temperature
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. filtrationthe precipitated crystals were filtered off
  4. customThe filtrate was evaporated under reduced pressure
  5. customthe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-8f4606f8f40f4bbbbb515a71ce510246
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04888044

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