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Diisopropylethylamine → 3-{[2-[2,6-Bis(isopropyl)phenoxycarbonyl]-benzoyl]amino}-propanoic Acid

HRID 2103790
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HRID 2103790 반응식
[CH:1]([C:4]1[CH:22]=[CH:21][CH:20]=[C:19]([CH:23]([CH3:25])[CH3:24])[C:5]=1[O:6][C:7]([O:9]C1C=CC=CC=1C(O)=O)=O)([CH3:3])[CH3:2].Cl.C([O:31][C:32](=[O:36])[CH2:33][CH2:34][NH2:35])(C)(C)C.C(N([CH:43]([CH3:45])[CH3:44])CC)(C)C>CN(C=O)C.C(OCC)(=O)C>[CH:23]([C:19]1[CH:20]=[CH:21][CH:22]=[C:4]([CH:1]([CH3:2])[CH3:3])[C:5]=1[O:6][C:7]([C:44]1[CH:43]=[CH:45][CH:2]=[CH:1][C:4]=1[C:5]([NH:35][CH2:34][CH2:33][C:32]([OH:31])=[O:36])=[O:6])=[O:9])([CH3:24])[CH3:25]
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참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 16218890Tert-butyl 3-aminopropanoate hydrochlorideHCID 211100152-[2,6-Bis(isopropyl)phenoxycarbonyloxy]-benzoic Acid

생성물 1

HCID 114180783-{[2-[2,6-Bis(isopropyl)phenoxycarbonyl]-benzoyl]amino}-propanoic Acid수율 8%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To a solution of crude compound (106) (0.4 g, 1.1 mmol) from above and beta-alanine tert-butyl ester hydrochloride (0.2 g, 1.1 mmol) in DMF (5 mL) was added diisopropylethylamine (0.41 mL, 2.3 mmol) followed by O-(benotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (0.44 g, 1.1 mmol). The resulting reaction mixture was stirred at room temperature for 14 h, diluted with ethyl acetate (50 mL), washed with 10% aqueous citric acid solution (30 mL), followed by saturated aqueous NaHCO3 solution (30 mL) and brine (2×20 mL). The organic phase was dried over MgSO4 and concentrated in vacuo. The crude residue was then dissolved in anhydrous dichloromethane (5 mL) and cooled to 0° C. before a solution of hydrochloric acid (1 mL, 4 N in dioxane) was added. The reaction was stirred for 2 h at 0° C. and the solvent was removed in vacuo. The crude residue was purified by preparative LC/MS to afford 50 mg (8% yield over three steps) of the title compound (103). 1H NMR (400 MHz, CDCl3): δ 6 7.85 (dd, J=7.6, 1.6 Hz, 1H), 7.51-7.48 (m, 1H), 7.34-7.13 (m, 5H), 3.72 (q, J=6.0 Hz, 2H), 3.13-3.10 (m, 2H), 2.67 (t, J=6.4 Hz, 2H), 1.25 (d, J=6.8 Hz, 12H). MS (ESI) m/z 414.3 (M+H+).

후처리

  1. customThe resulting reaction mixture
  2. washwashed with 10% aqueous citric acid solution (30 mL)
  3. dry with materialThe organic phase was dried over MgSO4
  4. concentrationconcentrated in vacuo
  5. dissolutionThe crude residue was then dissolved in anhydrous dichloromethane (5 mL)
  6. temperaturecooled to 0° C. before a solution of hydrochloric acid (1 mL, 4 N in dioxane)
  7. additionwas added
  8. stirringThe reaction was stirred for 2 h at 0° C.
  9. customthe solvent was removed in vacuo
  10. customThe crude residue was purified by preparative LC/MS

출처 및 근거

ORD 기록
ord-85c3aca3914c4ee3a286ecb86944c029
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576127B2

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