Ethanol → 4-(9-isopropyl-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-benzoic acid

HRID 2111351Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2111351
Cl[C:2]1[N:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10](=[O:13])[CH2:9][CH2:8][N:7]([CH:14]([CH3:16])[CH3:15])[C:6]=2[N:17]=1.[NH2:18][C:19]1[CH:27]=[CH:26][C:22]([C:23]([OH:25])=[O:24])=[CH:21][C:20]=1[O:28][CH3:29].C(O)C>Cl.O>[CH:14]([N:7]1[CH2:8][CH2:9][C:10](=[O:13])[N:11]([CH3:12])[C:5]2[CH:4]=[N:3][C:2]([NH:18][C:19]3[CH:27]=[CH:26][C:22]([C:23]([OH:25])=[O:24])=[CH:21][C:20]=3[O:28][CH3:29])=[N:17][C:6]1=2)([CH3:16])[CH3:15]

Komponenten

6

Edukt 3

HCID 702EthanolHCID 2880572486-69-3HCID 866175432-Chloro-9-isopropyl-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one

Produkt 1

HCID 686813864-(9-isopropyl-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-benzoic acidAusbeute 67,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 0.076 g (0.0003 mole) of 2-chloro-9-isopropyl-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-43), 0.060 g (0.00036 mole) of 4-amino-3-methoxy-benzoic acid, 0.5 mL of ethanol, 2 mL of water, and 2 drops of hydrochloric acid was heated at 100 degrees overnight. Upon cooling, a precipitate formed which was collected by filtration to give 0.078 g of 4-(9-isopropyl-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-benzoic acid (I-43a) as an off-white solid.

Aufarbeitung

  1. temperaturewas heated at 100 degrees overnight
  2. temperatureUpon cooling
  3. customa precipitate formed which
  4. filtrationwas collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-d123af84ae0a44229987c7cb6d7f246a
Quelldatensatz
uspto-grants-2009_04
Patentnummer
US07517873B2

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