HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosulfonyl isocyanate → HCID 10039065, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosulfonyl isocyanate | HCID 70918 | — |
| Reactant | 2-amino-5-benzylthiophene-3-carboxamide | HCID 3853457 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10039065 | HCID 10039065 | 67.6% |
Reaction Steps
Chlorosulfonyl isocyanate (0.09 mL, 1.03 mmol) was added dropwise under nitrogen to a solution of 2-amino-5-benzyl-thiophene-3-carboxylic acid amide (0.2 g, 0.86 mmol) in dry dichloromethane (9 mL) at 0° C. and. The temperature of the resulting stirred reaction mixture was slowly raised from 0° C. to room temperature over 1 h. Once the LC-MS showed no starting material remaining, the reaction was quenched with water (1 mL) and stirred for 10 additional min. The solvent was removed under vacuum and the residue was taken up into DMSO (2 mL) and purified utilizing a Gilson preparative HPLC to give the above titled compound as a light brown solid (0.16 g, 67%). LC-MS [M+H]+ m/z 276.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07375131B2 |
| Source dataset | uspto-grants-2008_05 |
| ORD ID | ord-1331ab375b15477d9425a53a85c4aae2 |
| Source note | uspto-grants-2008_05 |