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

HRID 2111336

Reaktionsgleichung

Reaktionsgleichung von HRID 2111336
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]([CH2:14][CH2:15][O:16][CH3:17])[C:6]=2[N:18]=1.[NH2:19][C:20]1[CH:28]=[CH:27][C:23]([C:24]([OH:26])=[O:25])=[CH:22][C:21]=1[O:29][CH3:30].C(O)C>Cl.O>[CH3:30][O:29][C:21]1[CH:22]=[C:23]([CH:27]=[CH:28][C:20]=1[NH:19][C:2]1[N:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10](=[O:13])[CH2:9][CH2:8][N:7]([CH2:14][CH2:15][O:16][CH3:17])[C:6]=2[N:18]=1)[C:24]([OH:26])=[O:25]

Komponenten

6

Edukt 3

HCID 702EthanolHCID 2880572486-69-3HCID 866175782-Chloro-9-(2-methoxy-ethyl)-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one

Produkt 1

HCID 687404513-methoxy-4-[9-(2-methoxy-ethyl)-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino]-benzoic acidAusbeute 68,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 0.108 g (0.0004 mole) of 2-chloro-9-(2-methoxy-ethyl)-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-40), 0.08 g (0.00048 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 0.11 g of 3-methoxy-4-[9-(2-methoxy-ethyl)-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino]-benzoic acid (I-40a) 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-50f08a3f19f641f5b4eb7e0bbb137a07
Quelldatensatz
uspto-grants-2009_04
Patentnummer
US07517873B2

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