Methanol → 3-(2-methoxyethoxy)azetidine hydrochloride

Temperature

70 °C

1-Chloroethyl chloroformate (102 μL, 0.9 mmol) was added to a solution of 1-benzhydryl-3-(2-methoxyethoxy)-azetidine (215 mg, 0.7 mmol) in 1,2-dichloroethane (3 mL) at room temperature. The reaction mixture was then heated up to 70° C. and stirred for 2.5 hours. After cooling down to room temperature, methanol (3 mL) was added and the reaction mixture was stirred overnight at 70° C. The mixture was then concentrated to dryness and the residue was triturated in pentane (2×15 mL) to give a yellow oil (109 mg, 90%) which was used in the next step without further purification.

1. temperatureAfter cooling down to room temperature
2. stirringthe reaction mixture was stirred overnight at 70° C
3. concentrationThe mixture was then concentrated to dryness
4. customthe residue was triturated in pentane (2×15 mL)

ORD record

ord-4e8ceae1c37745c795b13652c57703e7

Source dataset

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09321769B2