反応 #69630

反応方程式

tin

compound XXII

1,1-dimethyl-ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine

1,1-dimethyl-ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine

→

1,1-dimethyl-ethyl-(6-amino-2,3-dichlorobenzyl)glycine

反応条件

後処理

1. 1
   その他The catalyst is then removed by filtration
2. 2
   濃縮the filtrate concentrated
3. 3
   workup.ADDITIONdiluted with water
4. 4
   その他The organic phase is separated
5. 5
   濃縮concentrated
6. 6
   その他the crude material purified by low temperature recrystallization

実験手順

Where possible, the invention seeks to avoid the use of a tin-reagent to effect the reduction. Thus in another procedure according to the invention, 1,1-dimethyl-ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine (compound XXII) may also be catalytically hydrogenated using a metal or metal-based catalyst such as platinum, platinum oxide, rhodium, and palladium on carbon under hydrogen pressure. The catalyst is then removed by filtration and the filtrate concentrated, diluted with water and an organic solvent and basified using an alkali to a pH of about 9-10. The organic phase is separated and concentrated and the crude material purified by low temperature recrystallization to give 1,1-dimethyl-ethyl-(6-amino-2,3-dichlorobenzyl)glycine.

出典