HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 69960675, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Hydroxyphenyl hydrogen sulfate | HCID 3083879 | — |
| Reactant | HCID 53947371 | HCID 53947371 | — |
| Catalyst | ICE protocol 1 | HCID 56841950 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 69960675 | HCID 69960675 | — |
Reaction Steps
Whilst cooling externally with ice 1.377 g (7.998 mmol) of pyrocatechol sulfate was added to a solution of 2.000 g (3.974 mmol) of 1-(4-amino-3,5-dibromo-D-phenylalanyl)-4-(1-methyl-4-piperidinyl)piperazine and 0.61 mL (0.004 mmol) of triethylamine in 50 mL of dimethylformamide and the mixture was then stirred for 1 hour whilst still being cooled with ice and for 2 hours at room temperature. The reaction mixture was concentrated by evaporation in vacuo at a maximum bath temperature of +40° C., the residue was triturated with diethylether, dried in air and used in the next step without further purification. Yield: 2.68 g (100% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313097B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-1395aafb478a416db0c70ad3b21833be |
| Source note | uspto-grants-2001_11 |