HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid methylene chloride → HCID 23554372, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | HCID 23554393 | HCID 23554393 | — |
| Product | HCID 23554372 | HCID 23554372 | 68.3% |
Reaction Steps
3-(N′-(tert-Butoxycarbonyl)-L-alaninyl)amino-2,3-dihydro-1-(4,4,4-trifluorobutyl)-5-phenyl-1H-1,4-benzodiazepin-2-one (1.21 g, 2.27 mmol) was added to 50 mL of a stirring solution of 15% TFA/methylene chloride in one portion. After stirring 2 h, the reaction mixture was concentrated under reduced pressure and the residue was dissolved in 100 mL of methylene chloride. This solution was washed twice with saturated sodium bicarbonate, once with brine and then dried over sodium sulfate. Purification of the crude product using silica gel column chromatography (1-5% methanol/methylene chloride) gave 670 mg (68%) of a light pink foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06667305B1 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-7db86ae15b214f6e9a8b79713f7d87e7 |
| Source note | uspto-grants-2003_12 |