It's perfectly okay to do an ALTER DATABASE while the system is in use. All it will do is slow the responsiveness of the system somewhat during the time the disk space is being swept (Sybase writes nulls to each byte on the disk when new space is added to a database). However, this is no more intrusive than any other user doing a long query that requires a lot of IO.
Having the responsiveness go down a bit is a lot less disruptive than kicking everyone off and there's no advantage in terms of reliability or soundness of practice in booting off the users before expanding a DB.
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