HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → tert-Butyl [4-(hydroxymethyl)benzyl]carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-(((tert-Butoxycarbonyl)amino)methyl)benzoic acid | HCID 853605 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | tert-Butyl [4-(hydroxymethyl)benzyl]carbamate | HCID 2794813 | 100% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
LiAl4 (227 mg, 5.97 mmol) was slurried in a mixture of THF (5 mL) and dioxane (5 mL) and cooled to 0° C. under an atmosphere of N2. 4-(tert-Butoxycarbonylamino-methyl)-benzoic acid was dissolved in a mixture of THF (5 mL) and dioxane (5 mL) and added to the chilled solution drop-wise over 15 min. The reaction mixture was allowed to warm to r.t and stirred for 16 h. Water (1 mL) was added to the reaction mixture which was then filtered through celite. The filtrate was evaporated to dryness and the residue partitioned between EtOAc (25 mL) and water (25 mL). The aqueous layer was extracted with EtOAC (2×25 mL), the organic layers combined, dried (Na2SO4) and evaporated to dryness to afford the desired product (460 mg, 100%). m/z 260 [M++Na]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07939666B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-3d75535b970644e888c2fee780998178 |
| Source note | uspto-grants-2011_05 |