HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 13060078, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 13060114 | HCID 13060114 | — |
| Product | HCID 13060078 | HCID 13060078 | — |
Reaction Steps
3-hydroxy-5-methyl-2,3-dihydro-imidazo[2,1-b]thiazole-6-carboxylic acid ethyl ester (4.00 mmol) is added to POCl3 (9.3 mL), stirred at reflux for 3 h and concentrated in vacuo. Chloroform and ice-water are added successively and the mixture is neutralized by addition of Na2CO3. The layers are separated and the aq. layer is extracted with chloroform. The combined organic layers are dried over Na2SO4 and concentrated in vacuo to give the desired product which is purified by FC (heptane/EtOAc 1/1 to EtOAc). LC-MS: tR=0.66 min; [M+H]+=211.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063099B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-32e728b168ac4652be28013032e86911 |
| Source note | uspto-grants-2011_11 |