反応 #87891

反応方程式

3′-{N′-[1-(3,4-dimethylphenyl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]hydrazino}-2′-methoxybiphenyl-3-carboxylic acid

acetic acid

→

3′-{N′-[1-(3,4-dimethylphenyl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]hydrazino}-2′-hydroxybiphenyl-3-carboxylic acid

溶媒

hydrobromic acid

反応条件

後処理

1. 1
   温度heated
2. 2
   温度under reflux for about 60 hours
3. 3
   濃縮The reaction mixture was concentrated under vacuum to a thick residue
4. 4
   workup.ADDITIONWater (40 mL) was added
5. 5
   ろ過The mixture was filtered
6. 6
   その他to give an orange solid, which
7. 7
   洗浄was washed with water (25 mL)
8. 8
   その他dried in an oven at 55° C. about to about 60° C. for about 12 hours

実験手順

A solution of 3′-{N′-[1-(3,4-dimethylphenyl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]hydrazino}-2′-methoxybiphenyl-3-carboxylic acid (4 g), prepared as in Example 3, in 48% aqueous hydrobromic acid (35 mL) and glacial acetic acid (35 mL) was stirred and heated under reflux for about 60 hours. The reaction mixture was concentrated under vacuum to a thick residue. Water (40 mL) was added and basified to pH 7-8 using saturated solution of sodium bicarbonate (20 mL). The mixture was filtered to give an orange solid, which was washed with water (25 mL) and dried in an oven at 55° C. about to about 60° C. for about 12 hours.

出典