Diisopropylethylamine → 3-{1-[6-(4-Amino-3-methyl-5-nitro-phenoxy)-pyrimidin-4-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one

HRID 1846453Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1846453
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1.Cl[C:22]1[N:27]=[CH:26][N:25]=[C:24]([O:28][C:29]2[CH:34]=[C:33]([N+:35]([O-:37])=[O:36])[C:32]([NH2:38])=[C:31]([CH3:39])[CH:30]=2)[CH:23]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[NH2:38][C:32]1[C:33]([N+:35]([O-:37])=[O:36])=[CH:34][C:29]([O:28][C:24]2[N:25]=[CH:26][N:27]=[C:22]([N:17]3[CH2:18][CH2:19][CH:14]([N:10]4[CH2:9][CH2:8][C:7]5[CH:20]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]=5[NH:12][C:11]4=[O:13])[CH2:15][CH2:16]3)[CH:23]=2)=[CH:30][C:31]=1[CH3:39]

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 866639074-(6-Chloro-pyrimidin-4-yloxy)-2-methyl-6-nitro-phenylamine

Produkt 1

HCID 669782863-{1-[6-(4-Amino-3-methyl-5-nitro-phenoxy)-pyrimidin-4-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

496 mg (1.80 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one, 480 mg (1.71 mmol) 4-(6-chloro-pyrimidin-4-yloxy)-2-methyl-6-nitro-phenylamine and 0.697 mL (4.00 mmol) DIPEA were combined in 10.0 mL DMF and stirred overnight at RT. The reaction mixture was added to ice water, the precipitate formed was suction filtered, washed with water and dried under HV.

Aufarbeitung

  1. customthe precipitate formed
  2. filtrationfiltered
  3. washwashed with water
  4. customdried under HV

Quellen und Nachweise

ORD-Eintrag
ord-a98b26e15af84daa8ad17339cb4b199e
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08952014B2

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