Double ketole colorless benzofuryl ketone compound and its preparation
A technology of benzofuranone and compound, which is applied in the field of bisindole thermosensitive dyes and its preparation, can solve the problems such as the absence of polymer active groups and the absence of polymer monomer conditions
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example 1
[0041] Example 1: Preparation of 1-ethyl-2-methylindole-2'-carboxy-4'-nitro-3 phenone
[0042] In a 100 ml three-necked flask with mechanical stirring, a thermometer, and a reflux condenser, add 10.0 g (0.0628 moles) of 1-ethyl-2-methylindole and 30 ml of 1,2-dichloroethane, and add 14.5 g (0.075 mol) of 4-nitrophthalic anhydride was heated to reflux for 3 hours, the reaction mixture was cooled to room temperature, and the precipitate was vacuum filtered to obtain a khaki crude product. Wash with fresh 1,2-dichloroethane and anhydrous methanol, recrystallize from methanol, and dry to give bright yellow solid 1-ethyl-2-methylindole-2'-carboxy-4'-nitro -3 benzophenone 17.2 grams. Melting point: 199-201°C.
example 2
[0043] Example 2: Preparation of 3,3-bis[(1-ethyl-2-methyl)-3-indolyl]-6-nitrobenzofuranone
[0044]In a 100 ml three-necked flask with mechanical stirring, a thermometer, and a reflux condenser, 14.2 grams of the above-mentioned synthesized 1-ethyl-2-methylindole-2'-carboxy-4'-nitro-3 phenone ( 0.04 mol) and 7.64 g (0.048 mol) of 1-ethyl-2-methylindole were suspended in 50 ml of acetic anhydride. Stir and heat up to 50-60°C, keep warm for 3 hours, cool the reddish-brown turbid liquid to room temperature, pour the reaction mixture into 1000 ml of 5% sodium hydroxide solution, stir well, there is a yellow precipitate, cool, filter, and then use ethanol After washing and drying, 19.3 g of yellow solid was obtained. Recrystallize with ethanol, dry, obtain 3,3-bis[(1-ethyl-2-methyl)-3-indolyl]-6-nitrobenzofuranone (in general formula (II): R 1 = H; R 2 =H) 18.2 g. Melting point: 208-210°C.
[0045] A benzene solution of this product was spotted on a silica gel sheet as a pur...
example 3
[0046] Example 3: Preparation of 3,3-bis[(1-ethyl-2-methyl)-3-indolyl]-6-aminobenzofuranone
[0047] In 500 milliliters of four-necked flasks with mechanical stirring, thermometer and reflux condenser, add 40 grams (0.175 moles) of tin protochloride, 240 milliliters of 30% hydrochloric acid, heat and stir to dissolve, cool to below 40 ℃, add the above-mentioned 11 grams (0.0223 moles) of 3,3-bis[(1-ethyl-2-methyl)-3-indolyl]-6-nitrobenzofuranone, make the temperature not more than 40°C, and The reaction was carried out at this temperature for 7 hours until the reaction mixture changed from purple to a rose red suspension and cooled to room temperature. Diluted with 1200 milliliters of water, 10% sodium hydroxide solution to adjust the pH of the reaction solution to be 12-14. 500 milliliters of benzene extraction, combined organic phase and interlayer floc, washed with 5% sodium hydroxide solution, washed with water, The solvent was distilled off to obtain 9.8 g of a pale pink...
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