反应详情

To 180 mg of 1-(7-carboxy-7-hydroxymethylheptyl)imidazole hydrochloride (prepared in Example 6(b)) was added 2 or 3 drops of phosphoric acid, and the mixture was reacted under reduced pressure at 160° C. for 5 hours. The reaction mixture was purified by column chromatography on cellulose using a mixture of n-butanol, water and acetic acid (8:10:1), and the obtained fraction was adjusted to pH 8 with a 1 N solution of sodium hydride in order to remove the contaminated phosphoric acid, and the resulting crystals was removed off. The same purification by column chromatography on cellulose was repeated to give 78 mg of the title compound having the following physical characteristics:

1. customthe mixture was reacted under reduced pressure at 160° C. for 5 hours
2. customThe reaction mixture was purified by column chromatography on cellulose using
3. additiona mixture of n-butanol, water and acetic acid (8:10:1)
4. customto remove the contaminated phosphoric acid
5. customthe resulting crystals was removed off
6. customThe same purification by column chromatography on cellulose