Diisopropylethylamine → 1-(Isopropylsulfonyl)piperazine

A solution of 1-BOC-piperazine (0.617 mmol) and diisopropylethylamine (0.679 mmol) in 0.5 mL of methylene chloride was added to a 4 mL vial. Propane-2-sulfonyl chloride (0.679 mmol) was added to the vial, and the reaction mixture was shaken overnight at room temperature. When the reaction was complete, it was diluted with 1.5 mL of methylene chloride and extracted with 1 mL of 1N solution of hydrogen chloride followed by 1 mL of 10% potassium carbonate solution. The organic layer was concentrated in vacuo. The residue was dissolved in 0.5 mL of tetrahydrofuran and 4M solution of hydrogen chloride in dioxane (0.5 mL). The solution was shaken overnight at room temperature then concentrated in vacuo to give 1-(propane-2-sulfonyl)-piperazine.

1. extractionextracted with 1 mL of 1N solution of hydrogen chloride
2. concentrationThe organic layer was concentrated in vacuo
3. dissolutionThe residue was dissolved in 0.5 mL of tetrahydrofuran
4. stirringThe solution was shaken overnight at room temperature
5. concentrationthen concentrated in vacuo

ORDレコード

ord-828805a881f8485fbe7897d171c90c4a

出典データセット

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07425638B2