HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiophosgene → HCID 59646493, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiophosgene | HCID 10040 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Amino-3,5-dichloropyridine | HCID 89888 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59646493 | HCID 59646493 | 20.3% |
Reaction Steps
To a solution of 3,5-dichloropyridin-4-amine (4.0 g, 24.53 mmol) in DCM (20 mL), was added N-ethyl di-isopropyl amine (6.3 g, 48.83 mmol). The reaction mixture was stirred at RT for 30 minutes. The reaction mixture was cooled at 0° C. and thiophosgene (2.76 g, 24.00 mmol) was added drop wise. The reaction mixture was stirred at 0° C. to RT for 3-4 h. The reaction mixture was diluted with DCM and the obtained crude was purified by column chromatography to afford 1.0 g of the desired product. 1HNMR (DMSO-d6): δ 8.77 (s, 2H); MS [M+H]+: 205.20.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08519149B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-6e05c3a4ed6a46dabf279daa4b73223f |
| Source note | uspto-grants-2013_08 |