Dimethyl Sulfoxide → HCID 11172300、化合物

Oxalyl chloride (0.55 mL, 6.44 mmol) was added to a stirred solution of DMSO (0.92 mL, 12.87 mmol) in dry DCM (40 mL) at −78° C. and the reaction mixture was stirred for 15 minutes. Compound 22 (1 g, 4.29 mmol) dissolved in DCM (15 mL) was the added drop-wise and the reaction mixture was stirred at −78° C. for 1 hour. The reaction mixture was then quenched by adding Et3N (2.9 mL, 21.45 mmol) drop-wise and the solution was stirred at rt for 15 minutes. Water was then added to the solution and the reaction mixture was extracted with DCM. The organic layer was dried over Na2SO4, filtered and concentrated to yield crude compound 23 which was used as such for the next step.

1. stirringthe reaction mixture was stirred at −78° C. for 1 hour
2. customThe reaction mixture was then quenched
3. stirringthe solution was stirred at rt for 15 minutes
4. extractionthe reaction mixture was extracted with DCM
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated

ORDレコード

ord-da22b15ad2514d06aabfa36a25a7d013

出典データセット

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09044482B2