Eprosartan → HCID 86643031, Verbindung

HRID 1808666

Reaktionsgleichung

Reaktionsgleichung von HRID 1808666
[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]([OH:19])=[O:18])=[CH:15][CH:16]=2)[C:8](/[CH:20]=[C:21](/[C:28]([OH:30])=[O:29])\[CH2:22][C:23]2[S:27][CH:26]=[CH:25][CH:24]=2)=[CH:7][N:6]=1>C(O)(=O)C>[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]([OH:19])=[O:18])=[CH:15][CH:16]=2)[C:8](/[CH:20]=[C:21](/[C:28]([OH:30])=[O:29])\[CH2:22][C:23]2[S:27][CH:26]=[CH:25][CH:24]=2)=[CH:7][N:6]=1.[C:17]([O-:19])(=[O:18])[CH3:14]

Komponenten

3

Edukt 1

HCID 5281037Eprosartan

Produkt 1

HCID 86643031HCID 86643031, VerbindungAusbeute 105,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
27.5 °C

Versuchsvorschrift

Crude eprosartan free base (50 gm, HPLC purity: 98.2%) is added to acetic acid (200 ml) under stirring at 25-30° C., the contents are heated to 80° C., to the resulting mass is added activated carbon (5 gm) and then stirred for 1 hour. The mass is filtered through a hyflow bed and the bed washed with hot acetic acid (50 ml). The filtrate is cooled to 25-30° C., methylene chloride (750 ml) is added drop wise to the mass and then stirred for 24 hours at 25-30° C. The mass is cooled to 0-5° C. and then stirred for 2 hours. The material is filtered, washed with methylene chloride (43 ml) and then dried to give 30 gm of pure eprosartan acetate (HPLC purity: 99.82%).

Aufarbeitung

  1. temperaturethe contents are heated to 80° C., to the resulting mass
  2. additionis added activated carbon (5 gm)
  3. stirringstirred for 1 hour
  4. filtrationThe mass is filtered through a hyflow bed
  5. washthe bed washed with hot acetic acid (50 ml)
  6. temperatureThe filtrate is cooled to 25-30° C.
  7. additionmethylene chloride (750 ml) is added drop wise to the mass
  8. stirringstirred for 24 hours at 25-30° C
  9. temperatureThe mass is cooled to 0-5° C.
  10. stirringstirred for 2 hours
  11. filtrationThe material is filtered
  12. washwashed with methylene chloride (43 ml)
  13. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ed8e3126018241c48e617491aac762d5
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08361507B2

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