Hydroxyamine hydrochloride → HCID 53722706、化合物

反応式

C([O-])(=O)C.[Na+].Cl.[NH2:7]O.C(O[CH:12]=[C:13]([C:30]([C:32]1([CH3:35])[CH2:34][CH2:33]1)=[O:31])[C:14]([C:16]1[CH:21]=[CH:20][C:19]([S:22]([CH3:25])(=[O:24])=[O:23])=[CH:18][C:17]=1[C:26]([F:29])([F:28])[F:27])=[O:15])C>>[CH3:25][S:22]([C:19]1[CH:20]=[CH:21][C:16]([C:14]([C:13]2[CH:12]=[N:7][O:31][C:30]=2[C:32]2([CH3:35])[CH2:34][CH2:33]2)=[O:15])=[C:17]([C:26]([F:29])([F:28])[F:27])[CH:18]=1)(=[O:24])=[O:23]

参加物

反応物 3

HCID 443297Hydroxyamine hydrochloride

HCID 517045Sodium Acetate

HCID 54056056HCID 54056056、化合物

生成物 1

HCID 53722706HCID 53722706、化合物収率 90.3%

実験手順

Sodium acetate (1.0 g) was added to a stirring mixture of hydroxylamine hydrochloride (0.85 g) and 2-ethoxymethylene-1-(4-methylsulphonyl-2-trifluoromethylphenyl)-3-(1-methylcyclopropyl)-propane-1,3-dione (4.2 g) in industrial methylated spirit (200ml). The mixture was stirred at room temperature for 3 hours. The mixture was evaporated to dryness and then suspended in ethyl acetate (100 ml). The resultant suspension was washed with water (100 ml), dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness to give 4-(4-methylsulphonyl-2-trifluoromethylbenzoyl)-5-(1-methylcyclopropyl)isoxazole (compound 99, 3.5 g) as a white solid, m.p. 141°-142° C.