HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenol → HCID 86736852, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenol | HCID 996 | — |
| Reactant | Chlorosulfonyl isocyanate | HCID 70918 | — |
| Reactant | 2-Amino-4,6-dimethoxypyrimidine | HCID 118946 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 86736852 | HCID 86736852 | 76.7% |
Reaction Steps
To a well stirred solution of 1.6 g of chlorosulfonyl isocyanate in 7 ml of dry xylene at ambient temperature and pressure was added 0.9 g of phenol. The resulting mixture was heated to reflux temperature for 1.5 hours. The solvent was removed under reduced pressure to give a clear oil. The oil was diluted with 5 ml of methylene chloride and added to a cooled (ice-water bath) suspension of 1.5 g of 2-amino-4.6-dimethoxypyrimidine in 10 ml of methylene chloride. The solvent was removed under vacuum. The resultant oil was triturated with 1-chlorobutane and filtered to yield 2.6 g of white solid, m.p. 136°-139° C. The infrared spectrum showed characteristic absorption bands at 3150 cm-1, 1720 cm-1, 1625 cm-1, 1580 cm-1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04191553 |
| Source dataset | uspto-grants-1980_03 |
| ORD ID | ord-855a9dad1ec6493dbde0fc300dd79eb6 |
| Source note | uspto-grants-1980_03 |