HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl chloride → HCID 89726899, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | HCID 89726514 | HCID 89726514 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89726899 | HCID 89726899 | — |
Reaction Steps
To a solution of 3,4-dihydro-1H-pyrrolo[2,1-c][1,4]thiazine-8-carboxylic acid ethyl ester (Comp. No. 2c) (0.5 g, 2.37 mmol) in anhydrous dichloromethane (1.7 ml) was added trichloro-acetyl chloride (1.08 g, 5.9 mmol). The resulting mixture was stirred overnight at room temperature, after which a second portion of trichloro-acetyl chloride (0.43 g, 2.37 mmol) was added. The resulting mixture was stirred for 4 h, and then evaporated to dryness. The crude product was purified by silica gel chromatography (eluting with 5 to 50% ethyl acetate in heptane) to give 0.592 g of 6-(2,2,2-Trichloro-acetyl)-3,4-dihydro-1H-pyrrolo[2,1-c][1,4]thiazine-8-carboxylic acid ethyl ester. LC/MS (method 4): Rt=1.41 min; m/z=356.09 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09284333B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-be039add46e04409809ae783e79f12d0 |
| Source note | uspto-grants-2016_03 |