HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-[2-({[(9H-fluoren-9-yl)methoxy]carbonyl}amino)acetamido]benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-Aminobenzoic Acid | HCID 7419 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Fmoc-Gly-Cl | HCID 11758879 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-[2-({[(9H-fluoren-9-yl)methoxy]carbonyl}amino)acetamido]benzoic acid | HCID 66966726 | 43% |
Reaction Steps
A solution of 3-aminobenzoic acid (0.5 g; 3.8 mmol) and N-ethyldiisopropylamine (DIEA) (0.64 mL; 3.8 mmol) in THF (20 mL) was added dropwise to a solution of Fmoc-glycine chloride (1.2 g; 4.0 mmol) (3) in THF (10 mL) and CH2Cl2 (10 mL). After 24 h stirring at room temperature 1 M HCl (50 mL) was added (final pH: 1.5). The precipitate was filtered, washed with H2O (2×100 mL), vacuum dried and crystallised from CHCl3/CH3OH (1:1) to give B as a white solid (0.7 g; 1.6 mmol). Yield 43%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07611692B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-b361f265b5dd41ddb6320f9ca05cbd5e |
| Source note | uspto-grants-2009_11 |