HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfate decahydrate → N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | N-(2,6-dichloro-4-cyanophenyl)acetamide | HCID 2735977 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamide | HCID 58962993 | 30% |
Reaction Steps
Step B (2): To a solution of 4-acetamido-3,5-dichloro-benzonitrile (114 mg, 0.5 mmol) in 5 mL of THF was added lithium aluminum hydride (120 mg, 3.2 mmol) in one portion and the resulting mixture was stirred for 3 h. Sodium sulfate decahydrate (1 g, 3.2 mmol) was added in one portion and the mixture was stirred for 30 min. The solid was filtered off and the filtrate was concentrated. The residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzylamine (35 mg, 30%). 1H NMR (500 MHz, CD3OD): δ 7.46 (s, 2 H), 3.78 (s, 2H), 2.18 (s, 3 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07390925B2 |
| Source dataset | uspto-grants-2008_06 |
| ORD ID | ord-cc504b15272a48c7a93affceaa977dc8 |
| Source note | uspto-grants-2008_06 |