تفاعل #11804

معادلة التفاعل

(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

المردود 84.1%

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

المردود 84.1%

المذيبات

dichloromethane

trifluoroacetic acid

ظروف التفاعل

المعالجة

1. 1
   تركيزconcentrated
2. 2
   workup.ADDITIONThe resulting residue was diluted with dichloromethane
3. 3
   أخرىthe excess trifluoroacetic acid was quenched with saturated aqueous sodium carbonate
4. 4
   استخلاصextracted one time with dichloromethane/methanol (1:1)
5. 5
   تجفيفThe combined organic layers were dried over magnesium sulfate
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated

الإجراء التجريبي

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).

المصدر