Ethyl Acetate → 3-(Cyclopropyl(2,6-dichloropyrimidin-4-yl)amino)propan-1-ol

HRID 930801Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 930801
[CH:1]1([NH:4][CH2:5][CH2:6][CH2:7][OH:8])[CH2:3][CH2:2]1.CCN(C(C)C)C(C)C.[Cl:18][C:19]1[N:24]=[C:23](Cl)[CH:22]=[C:21]([Cl:26])[N:20]=1.CCOC(C)=O>CN(C)C=O>[CH:1]1([N:4]([C:23]2[CH:22]=[C:21]([Cl:26])[N:20]=[C:19]([Cl:18])[N:24]=2)[CH2:5][CH2:6][CH2:7][OH:8])[CH2:3][CH2:2]1

Komponenten

6

Edukt 4

HCID 8857Ethyl AcetateHCID 773782,4,6-TrichloropyrimidineHCID 81531DiisopropylethylamineHCID 545472183-(Cyclopropylamino)propan-1-ol

Produkt 1

HCID 903031303-(Cyclopropyl(2,6-dichloropyrimidin-4-yl)amino)propan-1-olAusbeute 23,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of 3-(cyclopropylamino)propan-1-ol (7 g, 60.8 mmol) and Hunig's base (31.8 mL, 182 mmol) in N,N-dimethylformamide (20 mL), was added 2,4,6-trichloropyrimidine (7.10 mL, 60.8 mmol), stirred for 3 h at 0° C. Then, EtOAc (150 mL) was added, and the organic phase was washed with water, brine, dried over Na2SO4, and concentrated. Purification via FC afforded the title compound (3.8 g).

Aufarbeitung

  1. washthe organic phase was washed with water, brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customPurification via FC

Quellen und Nachweise

ORD-Eintrag
ord-06fbd6224ace4d6caecebf135a66ebc8
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09296755B2

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