HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuryl chloride → HCID 58934907, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | HCID 58934586 | HCID 58934586 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58934907 | HCID 58934907 | 53.1% |
Reaction Steps
To a mixture of 100 mg (0.35 mmol) of 6-ethyl-7-hydroxy-2-(trifluoromethyl)-2H-chromene-3-carboxylic acid in 5 mL of anhydrous dichloromethane was added dropwise a solution of 0.42 mL (1.0 M in dichloromethane, 0.42 mmol) sulfuryl chloride. The resulting solution was stirred at room temperature for one hour. The sample was concd and the residue purified on a silica gel column with ethyl acetate:hexane: acetic acid to give 60 mg (52%) of a light yellow solid: 1H NMR(CDCl3/400 MHz) 7.71(s, 1H), 6.71(s, 1H), 5.99(s, 1H), 5.65(q, J=6.0 Hz, 1H), 2.38(m, 1H), 2.06(m, 1H), 0.84(t, J=7.6 Hz, 3H); MS (ESI+) 323.0 (M+1, 100); LCMS (ES−) 321 (M−H, 100); HRMS (ES−) m/z calcd for (M−1; C13H9ClF3O4) 321.0136, found 321.0118.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07259266B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-0ebf07a0cf94459c889931a9aa900441 |
| Source note | uspto-grants-2007_08 |