HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloroethyl chloroformate → HCID 69951033, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | HCID 86757787 | HCID 86757787 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69951033 | HCID 69951033 | — |
Reaction Steps
A solution of intermediate compound IV (1.0 eq) and Protol Sponge (Aldrich, 1.0 eq) in CH2Cl2 under N2 was cooled to 10° C. A solution of 1-chloroethyl chloroformate (1.5 eq) in CH2Cl2 was added in a dropwise fashion over 30 min, and the reaction was stirred for 2 h while warming to room temperature. The reaction mixture was then subjected to chromatography by vacuum filtration (SiO2:CH2Cl2/Acetone). The resulting white solid was then suspended in MeOH and refluxed for 30 min. The solvent was then removed in vacuo to afford the desired product as the hydrochloride salt (70% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06348472B1 |
| Source dataset | uspto-grants-2002_02 |
| ORD ID | ord-53a5e80415c74eaabeeb52fca374d84a |
| Source note | uspto-grants-2002_02 |