Diisopropylethylamine → HCID 68600587, Verbindung

To a solution of 3.1 g triphosgene and 2.3 ml 3,3,3-trifluoropropan-1-ol in 70 ml dichloromethane were added 9.0 ml DIPEA dropwise at 0° C. After 30 minutes 5.1 ml benzyl 1-piperazinecarboxylate and 34.5 ml DIPEA were added at 0° C. The reaction mixture was allowed to warm to RT overnight. Excess triphosgene was destroyed by adding a solution of 2.5 g NaOH in 200 ml water and stirring for 2 h. The layers were separated, the organic layer dried over MgSO4 and concentrated. The crude product thus obtained was purified by chromatography on silica using heptane/ethyl acetate 4/1 to 2/1 as eluent. Yield: 3.2 g.

1. customExcess triphosgene was destroyed
2. additionby adding a solution of 2.5 g NaOH in 200 ml water
3. customThe layers were separated
4. dry with materialthe organic layer dried over MgSO4
5. concentrationconcentrated

ORD-Eintrag

ord-cd03afd3438a4c6084d9770fcfbaf9df

Quelldatensatz

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08669266B2