Methyl chloroformate → HCID 68003946, compound

Temperature

0 °C

Into a 50 mL round-bottom flask was placed a solution of 1-1,4-dioxaspiro[4.5]decan-8-ylpropan-1-amine hydrochloride (as prepared in the previous step, 50 mg, 0.21 mmol, 1.00 equiv) in dichloromethane (10 mL) and TEA (42.8 mg, 0.42 mmol, 2.00 equiv). This was followed by the addition of methyl carbonochloridate (23.9 mg, 0.25 mmol, 1.20 equiv) dropwise with stirring at 0° C. The resulting solution was stirred overnight at room temperature. The reaction was then quenched by the addition of 20 mL of water. The resulting solution was extracted with 2×20 mL of dichloromethane. The organic layers were combined, dried over anhydrous sodium sulfate and concentrated under vacuum to give the title compound as a yellow oil.

1. customInto a 50 mL round-bottom flask was placed
2. stirringThe resulting solution was stirred overnight at room temperature
3. customThe reaction was then quenched by the addition of 20 mL of water
4. extractionThe resulting solution was extracted with 2×20 mL of dichloromethane
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under vacuum

ORD record

ord-973a8209ba854836a9c5bce449419485

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09062048B2