反応 #302893

反応方程式

((2,3-dimethylphenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride

sodium hydroxide

→

title compound

収率 99.6%

((2,3-dimethylphenyl)methyl)-1,3-thiazolin-2-ylamine

収率 99.6%

溶媒

diethyl ether

water

反応条件

後処理

1. 1
   workup.ADDITIONThe reaction mixture was poured into a separatory funnel
2. 2
   その他the organic phase was removed
3. 3
   抽出The aqueous phase was extracted with 100 mL of diethyl ether
4. 4
   抽出The organic extract
5. 5
   乾燥dried with sodium sulfite
6. 6
   ろ過filtered
7. 7
   濃縮The filtrate was concentrated under reduced pressure

実験手順

A mixture of 1.4 grams (0.034 mole) of sodium hydroxide in 100 mL of water was added to a stirred, cold (ice water bath) mixture of 8.0 grams (0.031 mole) of ((2,3-dimethylphenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride (Compound C11) in 100 mL of diethyl ether. The reaction mixture was allowed to warm to ambient temperature where it stirred for two hours. The reaction mixture was poured into a separatory funnel and the organic phase was removed and saved. The aqueous phase was extracted with 100 mL of diethyl ether. The organic extract was combined with the saved organic phase, dried with sodium sulfite and filtered. The filtrate was concentrated under reduced pressure to yield 6.8 grams of the title compound as a white solid, melting point 110-114° C. The NMR spectrum was consistent with the proposed structure.

出典