Ethanol → HCID 67154553、化合物

1-Chloroethylchloroformate (361 μL, 3.33 mmol) was added to a solution of 1-benzhydryl-3-(2-(thiophen-2-yl)ethoxy)azetidine (1.11 g, 3.17 mmol) in dichloromethane (15 mL) at room temperature. The reaction mixture was stirred overnight at room temperature, then 1 hour at 70° C. After cooling down to room temperature, ethanol (15 mL) was added and the reaction mixture was stirred at 70° C. for 1 hour. After concentration to dryness, the crude mixture was triturated in pentane (2×15 mL) to give a yellow oil (698 mg, quantitative) which was used in the next step without further purification.

1. custom1 hour
2. customat 70° C
3. temperatureAfter cooling down to room temperature
4. stirringthe reaction mixture was stirred at 70° C. for 1 hour
5. concentrationAfter concentration to dryness
6. customthe crude mixture was triturated in pentane (2×15 mL)
7. customto give a yellow oil (698 mg, quantitative) which
8. customwas used in the next step without further purification

ORDレコード

ord-47656b198f414038afa9dbfa211a07ca

出典データセット

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09051321B2