Chloroacetyl chloride → HCID 21072072, compound

Temperature

0 °C

To a suspension of glycine benzylester hydrochloride (25.2 g, 12.5 mmol, Aldrich) in CH2Cl2 (200 ml) was added a solution of K2CO3 (77 g, 55.8 mmol) in H2O (200 ml). The mixture was cooled to 0° C. and chloroacetylchloride (21.0 g, 18.6 mol, Aldrich) was added dropwise in 15 min. The mixture was warmed to room temperature and stirred for 2 h. The two layers were separated and the aqueous layer was extracted with CH2Cl2 (100 ml). The organic layers were combined and washed with H2O (100 ml), brine (100 ml), dried (MgSO4). Evaporation of solvent afforded a light yellowish glassy solid. This was triturated with 250 ml of hexane. The colorless solid was collected and dried to give 30.0 g of the material 1.

1. temperatureThe mixture was warmed to room temperature
2. customThe two layers were separated
3. extractionthe aqueous layer was extracted with CH2Cl2 (100 ml)
4. washwashed with H2O (100 ml), brine (100 ml)
5. dry with materialdried (MgSO4)
6. customEvaporation of solvent
7. customafforded a light yellowish glassy solid
8. customThis was triturated with 250 ml of hexane
9. customThe colorless solid was collected
10. customdried

ORD record

ord-5b35cbf1339c47418ada591a6aaa4290

Source dataset

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07160535B2