Trifluoroacetic acid → Mercaptoacetyl glycyl glycine

26.32 g (75.09 mmol) Carboxy methyl-t-butyl disulfide glycyl glycine t-butyl ester were dissolved in 233 ml TFA under N2-atmosphere. The resulting solution was stirred for 20 min at room temperature. TFA was evaporated under reduced pressure (5-10×10−2 mbar) and the resulting oil was dried under stirring for additional 2 h (5-10×10−2 mbar). After addition of 250 ml Et2O a white powder precipitated and the suspension was stirred for 3 h. The material was filtered off and resuspended in 100 ml Et2O. The resulting suspension was stirred over night, the product was filtered off and the material was dried at room temperature under reduced pressure yielding 20.46 g (92.5%) as a white powder.

1. customTFA was evaporated under reduced pressure (5-10×10−2 mbar)
2. customthe resulting oil was dried
3. stirringunder stirring for additional 2 h (5-10×10−2 mbar)
4. additionAfter addition of 250 ml Et2O a white powder
5. customprecipitated
6. stirringthe suspension was stirred for 3 h
7. filtrationThe material was filtered off
8. stirringThe resulting suspension was stirred over night
9. filtrationthe product was filtered off
10. customthe material was dried at room temperature under reduced pressure
11. customyielding 20.46 g (92.5%) as a white powder

ORDレコード

ord-181e0887fb2245448e98feba011f5457

出典データセット

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08491906B2