Acetyl chloride → HCID 68003941, compound

Temperature

0 °C

Into a 50 mL round-bottom flask were placed a solution of 1-1,4-dioxaspiro[4.5]decan-8-ylpropan-1-amine hydrochloride (as prepared in Example 104 Step B) (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 acetyl chloride (19.8 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 were 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-f733bca501df4800b6445975cc0bc7a7

Source dataset

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08518969B2