Hydrochloric Acid → Dapivirine HCl

HRID 1070953Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1070953
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[NH:10][C:11]1[CH:16]=[CH:15][N:14]=[C:13]([NH:17][C:18]2[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[CH:20][CH:19]=2)[N:12]=1.[ClH:26].CC(O)C>C(O)C>[ClH:26].[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[NH:10][C:11]1[CH:16]=[CH:15][N:14]=[C:13]([NH:17][C:18]2[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[CH:20][CH:19]=2)[N:12]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 214347Dapivirine

Produkt 1

HCID 22398432Dapivirine HClAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Compound (52) (0.0015 mol) was stirred in boiling ethanol (8 ml), 6 M HCl in 2-propanol (0.0015 mol) was added and the salt was allowed to crystallize out overnight at room temperature. The precipitate was filtered off, washed with 2-propanol and dried, yielding 0.47 g (86%) of 4-[[4-[(2,4,6-trimethyl-phenyl)amino]-2-pyrimidinyl]amino]benzonitrile hydrochloride (1:1) (compound 53).

Aufarbeitung

  1. additionwas added
  2. customto crystallize out overnight at room temperature
  3. filtrationThe precipitate was filtered off
  4. washwashed with 2-propanol
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c76458f32f4d43a7bb959fbe79074eb2
Quelldatensatz
uspto-grants-2005_06
Patentnummer
US06903213B2

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