반응 #11804

반응 방정식

(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

수율 84.1%

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

수율 84.1%

용매

dichloromethane

trifluoroacetic acid

반응 조건

후처리

1. 1
   농축concentrated
2. 2
   workup.ADDITIONThe resulting residue was diluted with dichloromethane
3. 3
   기타the excess trifluoroacetic acid was quenched with saturated aqueous sodium carbonate
4. 4
   추출extracted one time with dichloromethane/methanol (1:1)
5. 5
   건조The combined organic layers were dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

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).

출처