HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 54002974, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diethyl cyanophosphonate | HCID 76257 | — |
| Reactant | 4-(Trifluoromethyl)benzylamine | HCID 76804 | — |
| Reactant | HCID 54071754 | HCID 54071754 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 54002974 | HCID 54002974 | 84% |
Reaction Steps
To a solution of 5-(2,4-dioxothiazolidin-5-ylidene)methyl-2-methoxybenzoic acid (1.00 g) and 4-trifluoromethylbenzylamine (627 mg) in DMF (10 ml), diethyl cyanophosphate (615 mg) and triethylamine (370 mg) were added at room temperature in an argon atmosphere under stirring, and the mixture was stirred for 5 hours as it was. The reaction liquor was poured into ice water and the crystals deposited were collected by filtration, washed with water, and then dried to obtain 1.31 g (84%) of aimed compound as crystals. Further, these were recrystallized from ethanol to obtain purified aimed compound as yellow prismatic crystals. Melting point 210.0~211.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06030990 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-781676b8d58042b2bd7a5445d5c045e0 |
| Source note | uspto-grants-2000_02 |