反应详情

A solution of hydroxy-di-thiophen-2-yl-acetic acid (1S,2R,4S,7S)-7-({9-[(R)-2-(tert-butyldimethylsilanyloxy)-2-(8-hydroxy-2-oxo-1,2-dihydro-quinolin-5-yl)ethylamino]-nonyl}methylamino)bicyclo[2.2.1]hept-2-yl ester (72 mg, 0.087 mmol) and triethylamine trihydrofluoride (60 μL, 0.37 mmol) was stirred in THF/DCM (1:1, 2 mL) at ambient temperature overnight. The reaction mixture was neutralised with satd NaHCO3 (aq) and extracted with DCM. The organic layer was concentrated to dryness to afford a green/brown oil, which was purified by preparative HPLC (system 1, 15% B+1% B/min for 20 min, then 6% B/min for 10 min). The fractions containing pure product were concentrated, neutralised with satd NaHCO3 (aq), and extracted with THF. After concentration in vacuo a light brown oil was obtained.

1. extractionextracted with DCM
2. concentrationThe organic layer was concentrated to dryness
3. customto afford a green/brown oil, which
4. customwas purified by preparative HPLC (system 1, 15% B+1% B/min for 20 min
5. additionThe fractions containing pure product
6. concentrationwere concentrated
7. extractionextracted with THF
8. concentrationAfter concentration in vacuo a light brown oil
9. customwas obtained