HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfate decahydrate → tert-Butyl [4-(hydroxymethyl)benzyl]carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | Methyl 4-((((1,1-dimethylethoxy)carbonyl)amino)methyl)benzoate | HCID 14221817 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | tert-Butyl [4-(hydroxymethyl)benzyl]carbamate | HCID 2794813 | 85.1% |
Reaction Steps
Lithium aluminum hydride (5.21 g) was suspended in THF (243 ml). Then, a solution of the compound (24.3 g) obtained in Example 103-1 in THF (243 ml) was gradually added to the suspension over 50 minutes while stirring under ice-cooling, followed by stirring at room temperature for 1 hour. The reaction solution was added with sodium sulfate decahydrate and a 20% sodium hydroxide aqueous solution and then filtrated through Celite. The filtrate was concentrated under reduced pressure and dried under vacuum, thereby obtaining the subject compound (18.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176227B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-e58cf39c14454272ab1d04d153b8fee3 |
| Source note | uspto-grants-2007_02 |