2-氯-4-(二甲基氨基)苯甲醛

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Following a procedure similar to that described above in Example 1, part A, 36.6 g of 2-chloro-4-dimethylaminobenzaldehyde and 33.0 g of 4-dimethylaminobenzoic acid were interacted in acetic anhydride to obtain 52.1 g of 3-(2-chloro-4-dimethylaminophenyl)-6-dimethylaminophthalide (Formula I: R=CH3 ; X=Z=H; Y=2-Cl-4-(CH3)2NC6H3) as a red crystalline solid which melted at 159°-160° C.

反应条件: temp:22.01; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Following a procedure similar to that described above in Example 1, part A, 36.6 g of 2-chloro-4-dimethylaminobenzaldehyde and 33.0 g of 4-dimethylaminobenzoic acid were interacted in acetic anhydride to obtain 52.1 g of 3-(2-chloro-4-dimethylaminophenyl)-6-dimethylaminophthalide (Formula I: R=CH3 ; X=Z=H; Y=2-Cl-4-(CH3)2NC6H3) as a red crystalline solid which melted at 159°-160° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 36.8 g of 2-chloro-4-dimethylaminobenzaldehyde, 25 ml of 1-nitropropane and 20 g of ammonium acetate in 150 ml of 1-propanol is refluxed for 15 hours. The mixture is then poured into 1.5 l of water whereupon the compound separates as a viscous red oil. Recrystallization twice from aqueous acetic acid yields 5.0 g of the compound, melting at 90°-91°. Recrystallization twice from aqueous acetic acid

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 36.8 g of 2-chloro-4-dimethylaminobenzaldehyde, 18 ml of nitroethane and 15 g of ammonium acetate in 150 ml of absolute ethanol is refluxed for 2 hours. The mixture is then poured into 1.5 l of water, whereupon the compound separates as a viscous red oil, which crystallizes on scratching. Recrystallization from ethanol yields 18.0 g of the compound, melting at 93°-94°. crystallizes Recrystallization from ethanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Following a procedure similar to that described above in Example 1, part A, 36.6 g of 2-chloro-4-dimethylaminobenzaldehyde and 33.0 g of 4-dimethylaminobenzoic acid were interacted in acetic anhydride to obtain 52.1 g of 3-(2-chloro-4-dimethylaminophenyl)-6-dimethylaminophthalide (Formula I: R=CH3 ; X=Z=H; Y=2-Cl-4-(CH3)2NC6H3) as a red crystalline solid which melted at 159°-160° C.