Diisopropylethylamine → HCID 67331064, 화합물

HRID 1896795노트

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HRID 1896795 반응식
[F:1][C:2]([F:8])([F:7])[CH2:3][C:4](O)=[O:5].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(C(C)C)CC)(C)C.[C:42]1([C:48]2[O:49][C:50]3[CH:56]=[CH:55][C:54]([NH2:57])=[CH:53][C:51]=3[CH:52]=2)[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1>ClCCl.C(OCC)(=O)C>[C:42]1([C:48]2[O:49][C:50]3[CH:56]=[CH:55][C:54]([NH:57][C:4](=[O:5])[CH2:3][C:2]([F:8])([F:7])[F:1])=[CH:53][C:51]=3[CH:52]=2)[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=1

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 27779723,3,3-Trifluoropropionic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 167651722-Phenyl-1-benzofuran-5-amine

생성물 1

HCID 67331064HCID 67331064, 화합물수율 29.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

To 3,3,3-trifluoropropanoic acid (136 mg, 1.06 mmol) in dry dichloromethane (10 mL) was added HATU (468 mg, 1.23 mmol) and diisopropylethylamine (580 μL, 3.35 mmol). The mixture was then stirred at room temperature for 10 min. 2-phenylbenzofuran-5-amine (234 mg, 1.12 mmol) was then added and the resulting mixture was stirred at room temperature for 48 h. Ethyl acetate was added and the organic layer was washed once with saturated aqueous water. The combined organic layers were dried over anhydrous MgSO4 and evaporated. The resulting solid was purified by column chromatography eluting using a gradient (ethyl acetate/hexanes 1:3 v/v to ethyl acetate/hexanes 1:1 v/v) followed by trituration in ethyl acetate to afford 99.3 mg (28%) of the title compound (LCMS RT=6.62 min)

후처리

  1. stirringthe resulting mixture was stirred at room temperature for 48 h
  2. washthe organic layer was washed once with saturated aqueous water
  3. dry with materialThe combined organic layers were dried over anhydrous MgSO4
  4. customevaporated
  5. customThe resulting solid was purified by column chromatography
  6. washeluting

출처 및 근거

ORD 기록
ord-07da71ba7d574f3cbd8def2a87ffe4a8
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518980B2

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