HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178486154, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | HCID 178527435 | HCID 178527435 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178486154 | HCID 178486154 | — |
Reaction Steps
To a solution of 1H-imidazole-4-sulfonyl chloride (0.5 g, 3.0 mmol; Matrix Scientific, Columbia, S.C.) in dichloromethane (10 mL) was added dimethylamine hydrochloride (0.245 g, 3.0 mmol) and triethylamine (1.3 mL, 9.0 mmol) at room temperature. The mixture was stirred for 16 hours at room temperature. TLC (petroleum ether/ethyl acetate=0:1) indicated the reaction was complete. The reaction mixture was washed with aq. ammonium chloride (30 mL) and extracted with dichloromethane: methanol=4:1 (3×50 mL). The combined organic phases were concentrated and precipitated from methanol to afford (I-35a) (0.36 g, 68.2%) as a white solid; 1H NMR (400 MHz, CD3OD): δ 7.74 (1H), 7.61 (1H), 2.68 (6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977367B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-073e4e513f0c4947bd13e854ead963db |
| Source note | uspto-grants-2011_07 |