Losartan → Losartan calcium

HRID 917006

Reaktionsgleichung

Reaktionsgleichung von HRID 917006
[CH3:1][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=3[C:23]3[N:27]=[N:26][NH:25][N:24]=3)=[CH:15][CH:16]=2)[C:8]([CH2:28][OH:29])=[C:7]([Cl:30])[N:6]=1.[OH-].[Ca+2:32].[OH-].CCCCCCC>C(O)(C)C>[CH3:1][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=3[C:23]3[N:27]=[N:26][NH:25][N:24]=3)=[CH:13][CH:12]=2)[C:8]([CH2:28][OH:29])=[C:7]([Cl:30])[N:6]=1.[Ca:32]

Komponenten

5

Edukt 3

HCID 3961LosartanHCID 8900HeptaneHCID 6093208Calcium Hydroxide

Produkt 1

HCID 69163274Losartan calciumAusbeute 160 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

To 40.81 g losartan of Example 1 in 235 ml i-propanol, 3.92 g calcium hydroxide were added, and it was stirred at reflux temperature for 1 hour, and hot filtered. 410 ml n-heptane were added to the filtrate and cooled to room temperature. The solvent was decanted from a resinous residue, and 820 ml n-heptane were added. It was stirred until a white solid crystallized. It was filtered, washed with 110 ml n-heptane, and dried in vacuo at 50° C. to yield 39.2 g losartan calcium.

Aufarbeitung

  1. temperatureat reflux temperature for 1 hour
  2. customThe solvent was decanted from a resinous residue, and 820 ml n-heptane
  3. additionwere added
  4. stirringIt was stirred until a white solid
  5. customcrystallized
  6. filtrationIt was filtered
  7. washwashed with 110 ml n-heptane
  8. customdried in vacuo at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-c757dcba4cd44316b696e8f6d415b1d5
Quelldatensatz
uspto-grants-2007_09
Patentnummer
US07271269B2

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