反応 #569308

反応方程式

D-(+)-glucosamine hydrochloride

triethylamine

ethyl trifluoroacetate

→

N-Trifluoroacetylglucosamine

溶媒

methanol

反応条件

後処理

1. 1
   温度cooling
2. 2
   濃縮At the end of this time, the mixture was concentrated by evaporation under reduced pressure
3. 3
   workup.ADDITIONbenzene (250 ml twice) and ethyl acetate (250 ml) were repeatedly added to the residue, which
4. 4
   濃縮was then concentrated by evaporation under reduced pressure
5. 5
   その他finally dried sufficiently in vacuo
6. 6
   その他The whole of the resulting crude trifluoroacetyl compound was used in the subsequent step (b) without purification

実験手順

160 g (0.742 mole) of D-(+)-glucosamine hydrochloride were dissolved in 2200 ml of methanol (99.6% purity), and 187.9 g (1.86 mole) of triethylamine were added to the resulting solution. 115.9 g of ethyl trifluoroacetate were then added dropwise to the resulting mixture, whilst ice-cooling, after which the mixture was stirred overnight at room temperature. At the end of this time, the mixture was concentrated by evaporation under reduced pressure, and then benzene (250 ml twice) and ethyl acetate (250 ml) were repeatedly added to the residue, which was then concentrated by evaporation under reduced pressure and then finally dried sufficiently in vacuo. The whole of the resulting crude trifluoroacetyl compound was used in the subsequent step (b) without purification.

出典