Diisopropylethylamine → Ethyl (βR)-β-[(2-cyclopropyl-5-nitro-4-pyrimidinyl)amino]benzenepropanoate

HRID 2175201

Reaktionsgleichung

Reaktionsgleichung von HRID 2175201
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([CH:11]2[CH2:13][CH2:12]2)[N:3]=1.Cl.[CH2:15]([O:17][C:18](=[O:28])[CH2:19][C@@H:20]([NH2:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH3:16].CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C>[CH2:15]([O:17][C:18](=[O:28])[CH2:19][C@@H:20]([NH:27][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([CH:11]2[CH2:13][CH2:12]2)[N:3]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[CH3:16]

Komponenten

6

Edukt 3

HCID 81531DiisopropylethylamineHCID 2734508ethyl (3R)-3-amino-3-phenylpropanoate hydrochlorideHCID 56773419HCID 56773419, Verbindung

Produkt 1

HCID 58497407Ethyl (βR)-β-[(2-cyclopropyl-5-nitro-4-pyrimidinyl)amino]benzenepropanoate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 4-Chloro-2-cyclopropyl-5-nitro-pyrimidine (597 mg, 3 mmol) in DMF (10 ml) was added (R)-3-Amino-3-phenyl-propionic acid ethyl ester hydro chloride (582 mg, 3 mmol). The mixture was stirred on ice for 5 minutes the DIPEA (580 mg, 4.5 mmol) was added. The solution was stirred at room temperature for one hour. TLC showed disappearance of the starting material. The reaction mixture was diluted with ethyl acetate, washed with water, dried over MgSO4, filtered, evaporated to dryness to give oil, which was used as such for the next step.

Aufarbeitung

  1. additionwas added
  2. washwashed with water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customto give oil, which

Quellen und Nachweise

ORD-Eintrag
ord-9c9de4620c994ebb884a5a6e39191328
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09062056B2

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