HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 136347245, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | HCID 10314079 | HCID 10314079 | — |
| Reactant | 2-Amino-4-[(methoxymethoxy)methyl]-3-thiophenesulfonamide | HCID 57455187 | — |
| Product | HCID 136347245 | HCID 136347245 | 49% |
Reaction Steps
The product of Example 309G (37.5 mg, 0.15 mmol) and the product of Example 340D (50 mg, 0.15 mmol) were reacted in toluene (5 mL) at 100° C. for 3 hours. The reaction was concentrated under reduced pressure and the residue was purified by chromatography on silica gel using a Biotage-12 m column eluting with 2:98 methanol:dichloromethane to give the title compound as a yellow solid (36 mg, 49%). The sodium salt of the title compound was prepared according to the procedure of Example 1D. 1H NMR (300 MHz, DMSO-d6) δ 0.98 (d, J=6.99 Hz, 6 H), 1.57 (m, 2 H), 1.66 (m, 1 H), 4.45 (d, J=7.35 Hz, 2 H), 4.64 (s, 3 H), 4.71 (s, 3 H), 7.43 (s, 1 H), 7.46 (m, 1 H), 8.54 (d, J=6.99 Hz, 1 H), 8.87 (s, 1 H), 14.45 (br.s, 1 H). MS (DCI+) m/z 510 (M+NH4)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07902203B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-3f38e230f04746e7906f4a0ad04a2cfe |
| Source note | uspto-grants-2011_03 |