HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylcarbamoyl Chloride → HCID 22730503, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 22730650 | HCID 22730650 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22730503 | HCID 22730503 | — |
Reaction Steps
A solution of Example 183D (108 mg, 0.157 mmol) and triethylamine (45 μL, 0.32 mmol) in THF (2 mL) at room temperature was treated with dimethylcarbamic chloride (14 uL, 0.157 mmol), and stirred for 30 minutes. The mixture was purified by flash column chromatography on silica gel with 10:10:80 methanol/acetonitrile/ethyl acetate to provide the desired product. MS (ESI(−)) m/e 759 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ1.93 (m, 2H), 2.65 (t, 2H), 2.74 (s, 6H), 2.89 (m, 2H), 3.08 (m, 4H), 3.34 (m, 6H), 3.61 (m, 2H), 3.75 (s, 3H), 6.88 (d, 1H), 6.96 (s, 1H), 7.01 (d, 1H), 7.21 (m, 2H), 7.30 (t, 2H), 7.41 (m, 3H), 7.88 (d, 1H), 7.89 (d, 2H), 8.51 (d, 1H), 8.54 (t, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06720338B2 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-17128ca1eb84418da27f883847bdd6b5 |
| Source note | uspto-grants-2004_04 |