Reaktion #91561

Reaktionsgleichung

7-(2-(methyloxy)-6-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-2,3,4,5-tetrahydro-1H-3-benzazepine

Methanesulfonic acid

→

title compound

Ausbeute 82.0%

7-(2-(methyloxy)-6-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-2,3,4,5-tetrahydro-1H-3-benzazepine methanesulfonate

Ausbeute 82.0%

Lösungsmittel

2-propanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONvial containing a stir bar
2. 2
   workup.DISSOLUTION(solids dissolved)
3. 3
   SonstigeWhite solid precipitated after the first aliquot (43 μL)
4. 4
   workup.ADDITIONAfter all aliquots of the counterion solution were added
5. 5
   workup.STIRRINGthe suspension was stirred at 40° C. for 1 hr
6. 6
   TemperaturThe suspension was cooled to 5° C. at 0.5° C./min
7. 7
   workup.STIRRINGstirred for 15 min
8. 8
   SonstigeThe product was isolated on a Büchner funnel
9. 9
   Filtrationfilter paper
10. 10
    Sonstigeair-dried for 30 min
11. 11
    Sonstigedried at 40° C. under vacuum for 12 hrs

Vorschrift

7-(2-(methyloxy)-6-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-2,3,4,5-tetrahydro-1H-3-benzazepine (300.0 mg; 1.0 eq) was weighed into a 20-mL vial containing a stir bar and combined with 2-propanol (6.0 mL). The suspension was heated to 40° C. and stirred for 15 min (solids dissolved). Seeds of the methanesulfonate salt were added (˜1 mg). Methanesulfonic acid (3M in water; 1.1 eq.; 293.0 uL in aliquots: 43, 50, 100, and 100 μL) was added. White solid precipitated after the first aliquot (43 μL). The suspension was re-seeded with the methansulfonate salt (˜1 mg). After all aliquots of the counterion solution were added, the suspension was stirred at 40° C. for 1 hr. The suspension was cooled to 5° C. at 0.5° C./min and stirred for 15 min. The product was isolated on a Büchner funnel using #1 Whatman filter paper, air-dried for 30 min, and dried at 40° C. under vacuum for 12 hrs. The title compound was produced as a white crystalline powder. A yield of 82% was obtained.

Quelle