Hydrochloric Acid → HCID 68680492, Verbindung

HRID 639282Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 639282
ClC(Cl)(Cl)[C:3]([C:5]1[N:14]2[C:8]([CH2:9][N:10]([C:19](=[O:29])[CH2:20][O:21][C:22]3[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=3)[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13]2)=[CH:7][CH:6]=1)=[O:4].[OH-:32].[Na+].Cl>CC(C)=O>[Cl:28][C:25]1[CH:26]=[CH:27][C:22]([O:21][CH2:20][C:19]([N:10]2[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13][N:14]3[C:5]([C:3]([OH:4])=[O:32])=[CH:6][CH:7]=[C:8]3[CH2:9]2)=[O:29])=[CH:23][CH:24]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 160392192,2,2-trichloro-1-{10-[(4-chlorophenoxy)acetyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone

Produkt 1

HCID 68680492HCID 68680492, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

To a stirred solution of 2,2,2-trichloro-1-{10-[(4-chlorophenoxy)acetyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone (0.20 mmol) in acetone (1.2 mL) was added 0.15 mL of 2.5 N sodium hydroxide. After stirring for 20 hours the mixture was acidified with 2.0 N hydrochloric acid, extracted into ethyl acetate, washed with brine, and dried over anhydrous sodium sulfate. The solution was then evaporated and the residue purified by trituration with diethylether. The solid (0.066 g, 83%) was collected and dried, m.p. 168° C. MS [(+)ESI, m/z]: 395 [M+H]+ Anal. Calcd for C21H17CIN2O4: C, 63.56; H, 4.32; N, 7.06. Found: C, 63.66; H, 4.48; N, 6.86

Aufarbeitung

  1. extractionextracted into ethyl acetate
  2. washwashed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solution was then evaporated
  5. customthe residue purified by trituration with diethylether
  6. customThe solid (0.066 g, 83%) was collected
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7812427471d04d7e8cd24475e2c1de2b
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07691848B2

Notizen zur Reaktion

Wird geladen…