反応 #11804

反応方程式

(2-{2-[(2R)-2-carbamoylmethyl-4-(4-fluoro-benzyl)-piperazin-1-yl]-2-oxo-ethoxy}-5-chloro-phenoxy)-acetic acid tert-butyl ester

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title compound

収率 84.1%

(2-{2-[(2R)-2-Carbamoylmethyl-4-(4-fluoro-benzyl)-piperazin-1-yl]-2-oxo-ethoxy}-5-chloro-phenoxy)-acetic acid

収率 84.1%

溶媒

dichloromethane

trifluoroacetic acid

反応条件

後処理

1. 1
   濃縮concentrated
2. 2
   workup.ADDITIONThe resulting residue was diluted with dichloromethane
3. 3
   その他the excess trifluoroacetic acid was quenched with saturated aqueous sodium carbonate
4. 4
   抽出extracted one time with dichloromethane/methanol (1:1)
5. 5
   乾燥The combined organic layers were dried over magnesium sulfate
6. 6
   ろ過filtered
7. 7
   濃縮concentrated

実験手順

A solution of (2-{2-[(2R)-2-carbamoylmethyl-4-(4-fluoro-benzyl)-piperazin-1-yl]-2-oxo-ethoxy}-5-chloro-phenoxy)-acetic acid tert-butyl ester (0.070 g, 0.13 mmol) in dichloromethane (1 mL) and trifluoroacetic acid (0.10 mL) was stirred for 3.5 h and then concentrated. The resulting residue was diluted with dichloromethane and the excess trifluoroacetic acid was quenched with saturated aqueous sodium carbonate. The aqueous layer was neutralized with 0.1N hydrochloric acid and extracted one time with dichloromethane/methanol (1:1) and twice with ethyl acetate. The combined organic layers were dried over magnesium sulfate, filtered and concentrated to give the title compound (0.054 g, LRMS: 492.4, 494.4).

出典