HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 90332433, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 90332507 | HCID 90332507 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 90332433 | HCID 90332433 | 97.6% |
Reaction Steps
To a solution of ethyl 6-amino-5-bromo-2-cyclopropylbenzofuran-3-carboxylate (7 g, 22.5 mmol) in 1,4-dioxane and H2O (50 mL and 50 mL) was added LiOH.H2O (4.6 g, 112 mmol). The reaction mixture was refluxed for 2 hours, and then 400 mL H2O was added to the reaction mixture. After acidifying to pH 4˜5 with HCl, the resulting solid were filtered to give the product of 6-amino-5-bromo-2-cyclopropylbenzofuran-3-carboxylic acid (6.5 g, yield: 97%). 1H-NMR (400 MHz, MeOD) δ 7.86 (s, 1H), 6.85 (s, 1H), 4.31 (s, 2H), 2.93˜3.00 (m, 1H), 1.19˜1.22 (m, 2H), 1.13˜1.16 (m, 2H). MS (M+H)+: 296/298.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242998B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-84aa311212fe40abb668a6a60163cb35 |
| Source note | uspto-grants-2016_01 |