Boron trifluoride etherate → 6,7-Dihydroxy-2-(5-isoquinolinesulfonyl)-3-[(4-phenylpiperazinyl)methyl]-1,2,3,4-tetrahydroisoquinoline

To 314 mg of the amorphous compound obtained in Example 9, were added 2 ml of 1,2-ethanedithiol and 1 ml of boron trifluoride/ethyl ether, and the mixture was stirred at a room temperature for 18 hours. After the addition of saturated sodium bicarbonate aqueous solution, the reaction mixture was extracted twice with a mixture of chloroform and methanol (1:1), and the extract was dried over magnesium sulfate and concentrated under a reduced pressure to obtain a residue, which was then applied to a silica gel column and eluted with chloroform/methanol (50:1 to 20:1) to obtain 213 mg of the title compound in a colorless amorphous form.

1. extractionthe reaction mixture was extracted twice with a mixture of chloroform and methanol (1:1)
2. dry with materialthe extract was dried over magnesium sulfate
3. concentrationconcentrated under a reduced pressure
4. customto obtain a residue, which
5. washeluted with chloroform/methanol (50:1 to 20:1)

ORDレコード

ord-0c1d03dbfb5143ad8ea1cfcb08c5adee

出典データセット

uspto-grants-1993_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05245034