Diisopropylethylamine → HCID 25062676, Verbindung

HRID 657794Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 657794
Br[C:2]1[C:3]2[CH2:11][N:10]([C:12]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:13]=3[C:14]#[N:15])[CH2:9][CH2:8][C:4]=2[N:5]=[CH:6][N:7]=1.[NH2:21][C@@H:22]([C:26]1[CH:27]=[N:28][C:29]([C:32]([F:35])([F:34])[F:33])=[CH:30][CH:31]=1)[CH2:23][CH2:24][OH:25].C(N(CC)C(C)C)(C)C>C(#N)C>[Cl:20][C:17]1[CH:18]=[CH:19][C:12]([N:10]2[CH2:9][CH2:8][C:4]3[N:5]=[CH:6][N:7]=[C:2]([NH:21][C@@H:22]([C:26]4[CH:27]=[N:28][C:29]([C:32]([F:35])([F:33])[F:34])=[CH:30][CH:31]=4)[CH2:23][CH2:24][OH:25])[C:3]=3[CH2:11]2)=[C:13]([CH:16]=1)[C:14]#[N:15]

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 58103584(R)-3-amino-3-(6-(trifluoromethyl)pyridin-3-yl)propan-1-olHCID 598406952-(4-bromo-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-5-chlorobenzonitrile

Produkt 1

HCID 25062676HCID 25062676, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A reaction mixture of 2-(4-bromo-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-5-chlorobenzonitrile (35 mg, 0.10 mmol) and (R)-3-amino-3-(6-(trifluoromethyl)pyridin-3-yl)propan-1-ol (22 mg, 0.10 μmol) in acetonitrile (1 mL) and N,N-diisopropylethylamine (0.035 mL, 0.20 mmol) was subjected to microwave irradiation at 200° C. for 2 h. The reaction mixture was concentrated and the residue was purified by preparative HPLC (100×20.2 mm, C18 column; 30-70% CH3CN-water [10 mM Et2NH]) to yield an off-white solid.

Aufarbeitung

  1. customirradiation at 200° C. for 2 h
  2. concentrationThe reaction mixture was concentrated
  3. customthe residue was purified by preparative HPLC (100×20.2 mm, C18 column; 30-70% CH3CN-water [10 mM Et2NH])
  4. customto yield an off-white solid

Quellen und Nachweise

ORD-Eintrag
ord-2e4ccb1ed8a645d8bfe44a63671b03b1
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08076345B2

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