Diisopropylethylamine → HCID 68573992, 화합물

HRID 225496

반응식

HRID 225496 반응식
[CH2:1]([O:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][C:7]=1[NH:15][C:16]([NH2:18])=[NH:17])[CH:2]=[CH2:3].CN(C)[CH:21]=[CH:22][C:23]([C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)=O.C(N(C(C)C)C(C)C)C>C(O)CCC.C(OCC)(=O)C>[CH2:1]([O:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][C:7]=1[NH:15][C:16]1[N:18]=[C:23]([C:25]2[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=2)[CH:22]=[CH:21][N:17]=1)[CH:2]=[CH2:3]

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 5670331-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-oneHCID 178459007HCID 178459007, 화합물

생성물 1

HCID 68573992HCID 68573992, 화합물

시약·촉매·용매 2

HCID 2631-Butanol용매HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

A stirred mixture of {2-[(2-propenyloxy)-methyl]-5-nitro-phenyl}-guanidine (3.75 g, 15 mmol), 3-(dimethylamino)-1-(3-pyridinyl)-2-propen-1-one (2.60 g, 15 mmol) and ethyl diisopropylamine (2.6 mL, 15 mmol) in 1-butanol (50 mL) is heated at 120° C. for 20 h. The solvent is then evaporated off under reduced pressure to give a residue which is dissolved in ethyl acetate (100 mL). The resulting mixture is filtered (celite), washed with saturated aqueous sodium chloride (50 mL), dried (MgSO4), filtered and the solvent is evaporated off under reduced pressure to yield the crude product which is purified by column chromatography on silica gel, eluent ethyl acetate, and recrystallised from ethyl acetate-hexane to give the title compound as a yellow crystalline solid, m.p. 213-2150C.

후처리

  1. customThe solvent is then evaporated off under reduced pressure
  2. customto give a residue which
  3. filtrationThe resulting mixture is filtered (celite)
  4. washwashed with saturated aqueous sodium chloride (50 mL)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent is evaporated off under reduced pressure
  8. customto yield the crude product which
  9. customis purified by column chromatography on silica gel, eluent ethyl acetate
  10. customrecrystallised from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-56d4ff03fd554ab5ade9deb49f7d226d
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557105B2

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