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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → (R)-3-(4-[3-(3,5-Bis(trifluoromethyl)phenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoylamino]-2-hydroxypropionic acid ethyl ester

HRID 412431
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 412431
[F:1][C:2]([F:40])([F:39])[C:3]1[CH:4]=[C:5]([NH:13][C:14](=[O:38])[N:15]([CH2:28][C:29]2[CH:37]=[CH:36][C:32]([C:33](O)=[O:34])=[CH:31][CH:30]=2)[C:16]2[CH:21]=[CH:20][C:19]([CH:22]3[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:18][CH:17]=2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.ON1C2N=CC=CC=2N=N1.CCN=C=NCCCN(C)C.[CH2:62]([O:64][C:65](=[O:70])[C@H:66]([OH:69])[CH2:67][NH2:68])[CH3:63].C(N(C(C)C)CC)(C)C>CN(C=O)C.O>[CH2:62]([O:64][C:65](=[O:70])[C@H:66]([OH:69])[CH2:67][NH:68][C:33](=[O:34])[C:32]1[CH:31]=[CH:30][C:29]([CH2:28][N:15]([C:16]2[CH:17]=[CH:18][C:19]([CH:22]3[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]3)=[CH:20][CH:21]=2)[C:14]([NH:13][C:5]2[CH:6]=[C:7]([C:9]([F:10])([F:11])[F:12])[CH:8]=[C:3]([C:2]([F:1])([F:39])[F:40])[CH:4]=2)=[O:38])=[CH:37][CH:36]=1)[CH3:63]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 81531DiisopropylethylamineHCID 181649HOAtHCID 223110784-[3-(3,5-Bis(trifluoromethyl)phenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoic acidHCID 54263093ethyl (2R)-3-amino-2-hydroxypropanoate

Produkt 1

HCID 86586059
(R)-3-(4-[3-(3,5-Bis(trifluoromethyl)phenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoylamino]-2-hydroxypropionic acid ethyl ester
Ausbeute 101,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

4-[3-(3,5-Bis(trifluoromethyl)phenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoic acid (0.22 g, 0.39 mmol) was dissolved in DMF (3 mL) and 1-hydroxy-7-azabenzotriazole (0.06 g, 0.47 mmol) and EDAC (0.09 g, 1.2 mmol) were added. The mixture was stirred for 1.5 hour, and (R)-isoserine ethyl ester (0.10 g, 0.59 mmol) and diisopropylethylamine (0.10 mL, 0.59 mmol) in DMF (2 mL) were added. The mixture was stirred at room temperature for 16 hours. The reaction mixture was diluted with water (10 mL) and extracted with ethyl acetate (25 mL). The aqueous phase was extracted with ethyl acetate (10 mL). The combined organic phases were washed with hydrochloric acid (0.2 N, 3×10 mL) and water:saturated sodium chloride (1:1), dried (magnesium sulphate) and concentrated in vacuo. The residue was purified by column chromatography (35 g silica gel) using ethyl acetate and n-heptane (6:4) as eluent to afford 0.27 g of (R)-3-{4-[3-(3,5-bis(trifluoromethyl)phenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoylamino}-2-hydroxypropionic acid ethyl ester.

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for 16 hours
  2. extractionextracted with ethyl acetate (25 mL)
  3. extractionThe aqueous phase was extracted with ethyl acetate (10 mL)
  4. washThe combined organic phases were washed with hydrochloric acid (0.2 N, 3×10 mL) and water
  5. dry with materialsaturated sodium chloride (1:1), dried (magnesium sulphate)
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography (35 g silica gel)

Quellen und Nachweise

ORD-Eintrag
ord-7b8b7bb7c04d4619b1ae3906325fff34
Quelldatensatz
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06562807B2

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