HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Amino-2-chlorobenzoic acid → HCID 9917165, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Amino-2-chlorobenzoic acid | HCID 459315 | — |
| Reactant | HCID 69879159 | HCID 69879159 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 9917165 | HCID 9917165 | 81.9% |
Reaction Steps
DPP-Cl(68 μl) and TEA(50 μl) were added to a solution of 3-amino-2-chlorobenzoic acid (56 mg) in EtOAc (2 ml), and the mixture was stirred for one hour. After the addition of the compound obtained in Step 2 of Example 1 (141 mg) and TEA (50 μl), the mixture was stirred overnight. The reaction mixture was washed with 5% Na2CO3 (×2), 1N HCl, and 5% NaCl, dried over MgSO4. After filtration and concentration, the residue was purified by silica gel column chromatography (CH2Cl2—MeOH), and reprecipitated from a mixture of CH2Cl2 and n-hexane to obtain the title compound (153 mg, 81%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06673772B2 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-f5d2d4d27daf47ebb57762fface7bfcb |
| Source note | uspto-grants-2004_01 |