HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Thiazolemethanol, alpha-methyl- (7CI,9CI) → HCID 22220759, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Thiazolemethanol, alpha-methyl- (7CI,9CI) | HCID 9989295 | — |
| Reactant | O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine | HCID 11830845 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22220759 | HCID 22220759 | 80.1% |
Reaction Steps
O-(Mesitylenesulfonyl)hydroxylamine containing ca. 18% water (1.95 g, 1.60 g dry wt., ca. 7.4 mmole) was dissolved in dichloromethane (12 mL) and dried over Na2SO4 and filtered. This was added dropwise to a solution of 1-(2-thiazolyl)ethanol (0.8 g, 6.2 mmole) in dichloromethane (4 mL) at 0 C. After stirring an additional 12 hr at 4 C., the mixture was diluted with ether (13 mL) and stored at 4 C. for 1 hr. The supernatant was decanted from the syrupy precipitate, which was triturated with 1:1 dichloromethane-ether (10 mL) to yield a powder which was filtered out, washed with the same solvent, and dried to yield 1.71 g of the title compound, mp 105-107 C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06777557B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-bb2e18f27c12453ea828748c53964ac5 |
| Source note | uspto-grants-2004_08 |