HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 23507215, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Nitrobenzoyl chloride | HCID 8502 | — |
| Reactant | Thiomorpholine | HCID 67164 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23507215 | HCID 23507215 | 99.6% |
Reaction Steps
To a stirred solution of thiomorpholine (2.00 mL, 20 mmol) and Et3N (5.0 mL) in CH2Cl2 (60 mL) was added drop wise a solution of 4-nitrobenzoyl chloride (3.71 g, 20 mmol) in CH2Cl2 (50 mL) at 0° C. The reaction was allowed to stir at room temperature for over night and then washed with a saturated NaHCO3 solution (2×75 mL), and water (2×75 mL). The CH2Cl2 layer was dried (Na2SO4) and filtered and concentrated. Finally dried under high vacuum to afford 5.027 g (99%) of the 4-(4-nitrobenzoyl)thiomorpholine. 1H NMR (CDCl3, 300 MHz): δ 8.28 (d, 2H, J=9.0 Hz), 7.54 (d, 2H, J=8.7 Hz), 4.04 (br s, 2H), 3.61 (br s, 2H), 2.75 (br s, 2H), 2.57 (br s, 2H); LCMS (m/z): 253 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399472B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-fae1ac1640ee445cac2fa92919afe341 |
| Source note | uspto-grants-2013_03 |