反応 #1486673

反応方程式

1-(3,5-dichloro-2-hydroxyphenyl)-ethanone

3-methylbenzoic acid hydrazide

acetic acid

→

title material

収率 93.0%

3-methyl-benzoic acid [1-(3,5-dichloro-2-hydroxyphenyl)-ethylidene]-hydrazide

収率 93.0%

溶媒

EtOH

反応条件

後処理

1. 1
   温度was cooled to room temperature
2. 2
   その他to precipitate the product
3. 3
   ろ過The solid was collected via suction filtration
4. 4
   洗浄rinsed with H2O

実験手順

A suspension of 1-(3,5-dichloro-2-hydroxyphenyl)-ethanone (0.100 g, 0.49 mmol), 3-methylbenzoic acid hydrazide (0.069 g, 0.46 mmol), and glacial acetic acid (0.3 mL) in EtOH (3 mL) was heated to 60° C. for 4 h The reaction mixture was cooled to room temperature to precipitate the product. The solid was collected via suction filtration and rinsed with H2O to furnish the title material as a yellow solid (0.144 g, 93%): mp 221-223° C.; 1H NMR (400 MHz, DMSO) δ 14.48 (s, 1H), 11.54 (s, 1H), 7.79-7.72 (m, 2H), 7.68 (d, J=2.5 Hz, 1H), 7.64 (d, J=2.4 Hz, 1H), 7.47-7.42 (m, 2H), 2.52 (s, 3H), 2.41 (s, 3H); ESIMS m/z 337 ([M+H]+), 335 ([M−H]−).

出典