HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 61636-46-2
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | 2-Hydroxybenzonitrile | HCID 11907 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 61636-46-2 | HCID 136072557 | 35% |
Reaction Steps
Acetyl chloride (6.0 g, 76.4 mmol) was added drop-wise to methanol (10 mL) over 30 min. The temperature was kept at 20° C. by cooling the mixture in a water bath. After the addition of acetyl chloride, the solution was stirred for 2 h at room temperature. o-Hydroxybenzonitrile (4.0 g, 33.61 mmol) was added followed by toluene (20 mL). The mixture was stirred at room temperature under an argon atmosphere for 4 days. The precipitate was filtered and washed with toluene. After drying under high vacuum, 2-hydroxy-benzimidic acid methyl ester hydrochloride (2.2 g, 35%) was isolated as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07491728B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-db03c36d0b6246949dbcf50698db2d00 |
| Source note | uspto-grants-2009_02 |