Hydrochloric Acid → 6-[4-(2-Oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylic acid

HRID 74503Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 74503
[O:1]=[C:2]1[N:8]([CH:9]2[CH2:14][CH2:13][N:12]([C:15]3[N:20]=[CH:19][N:18]=[C:17]([C:21]([O:23]CC)=[O:22])[CH:16]=3)[CH2:11][CH2:10]2)[CH2:7][CH2:6][C:5]2[CH:26]=[CH:27][CH:28]=[CH:29][C:4]=2[NH:3]1.C(O)C.[OH-].[Na+].Cl>O>[O:1]=[C:2]1[N:8]([CH:9]2[CH2:10][CH2:11][N:12]([C:15]3[N:20]=[CH:19][N:18]=[C:17]([C:21]([OH:23])=[O:22])[CH:16]=3)[CH2:13][CH2:14]2)[CH2:7][CH2:6][C:5]2[CH:26]=[CH:27][CH:28]=[CH:29][C:4]=2[NH:3]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 702Ethanol2×HCID 14798Sodium HydroxideHCID 58386764Ethyl 6-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylate

Produkt 1

HCID 583864046-[4-(2-Oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

590 mg (1.49 mmol) ethyl 6-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylate, 20 mL ethanol, 1 mL water and 1 mL (4.0 mmol) of a 4M NaOH solution were stirred for 2 h at RT. The reaction mixture was diluted with water until the precipitate had dissolved. 1 mL of a 4M hydrochloric acid solution were added and the ethanol was eliminated i. vac. The reaction mixture was stirred for 30 min at RT, the precipitate was suction filtered and dried at 50° C. in the CAD.

Aufarbeitung

  1. dissolutionhad dissolved
  2. filtrationfiltered
  3. customdried at 50° C. in the CAD

Quellen und Nachweise

ORD-Eintrag
ord-bbc93f1415f8483fa6db930c91c452c8
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829006B2

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