Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 39235406 | HCID 39235406 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 83382924 | HCID 83382924 | — |
Reaction Steps
1.09 g (7.1 mmol) of 4-fluoro-N1,N1-dimethylbenzene-1,3-diamine followed by 4.6 cm3 of pyridine are added, at a temperature in the region of 5° C., under an argon atmosphere, to 2.82 g (9.5 mmol) of triphosgene in solution in 150 cm3 of dichloromethane. After stirring for 18 hours at a temperature in the region of 20° C., the reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa), to give a residue which is triturated in 40 cm3 of tetrahydrofuran. After filtration, a solution of 5-dimethylamino-2-fluorophenyl isocyanate in approximately 0.14 N tetrahydrofuran is obtained, which solution is used directly in the subsequent step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07566736B2 |
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| Source dataset | uspto-grants-2009_07 |
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| ORD ID | ord-ebf4f01a7e7a4e6ba4b2016398b927a3 |
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| Source note | uspto-grants-2009_07 |
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