HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 71622430, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 131734307 | HCID 131734307 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 71622430 | HCID 71622430 | 5.4% |
Reaction Steps
Trifluoroacetic acid (0.44 g, 3.89 mmol) is added to the tert-butyl 2,2′-({[2-(2-hydroxyethoxy)ethyl]imino}bis[pentane-5,1-diyloxybenzene-4,1-diyl(2-methylindolizine-1,3-diyl)carbonyl(2,4-dioxo-1,4-dihydroquinazoline-7,3(2H)-diyl)])diacetate (0.50 g, 0.39 mmol) in suspension in 4 mL of a DCM/MeOH mixture (1/1). The solution is stirred for 8 h at ambient temperature. The reaction mixture is run into water. The precipitate formed is filtered off, washed with water then with ethanol, and dried under vacuum. Purification by preparative HPLC on Kromasil C18 10 μm reverse phase [A=H2O/(CH3COONH4 0.1 M) 90/10; B=CH3CN/(CH3COONH4 0.1 M) 90/10, gradient A/B: 70/30 to 56/44] gives 25 mg (5%) of a yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09206177B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-1121ab3d2ce54b6cb11e5e8f78012d80 |
| Source note | uspto-grants-2015_12 |