反応 #5099

反応方程式

6-chloroacetylaminomethyl-2,3-dihydro-7-hydroxy-4-methyl-1H-indene-1-one

hydroxylamine hydrochloride

pyridine

ethanol

water

→

(2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6yl)-methylaminocarbonylmethylpyridinium chloride

反応条件

後処理

1. 1
   その他the solvent was removed by evaporation under a reduced pressure
2. 2
   その他to the residue thus obtained
3. 3
   温度cooled
4. 4
   その他crystallized
5. 5
   ろ過The crystals were collected by filtration
6. 6
   洗浄washed with water
7. 7
   その他recrystallized from water

実験手順

200 Grams of 6-chloroacetylaminomethyl-2,3-dihydro-7-hydroxy-4-methyl-1H-indene-1-one, 77.9 g of hydroxylamine hydrochloride, 300 ml of pyridine and 1,800 ml of ethanol were refluxed for 3 hours. After the reaction was completed, the solvent was removed by evaporation under a reduced pressure, then to the residue thus obtained was added 2 liters of water and the mixture was stirred vigorously, cooled and crystallized. The crystals were collected by filtration, washed with water, and recrystallized from water to obtain 167 g of (2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6yl)-methylaminocarbonylmethylpyridinium chloride. Colorless flake-like crystals. Melting point: 279° C. (Decomposed).

出典