HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-(1-(Tert-butoxycarbonyl)azetidin-3-yl)acrylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | tert-Butyl 3-[(1E)-3-ethoxy-3-oxoprop-1-en-1-yl]azetidine-1-carboxylate | HCID 10729697 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 3-(1-(Tert-butoxycarbonyl)azetidin-3-yl)acrylic acid | HCID 10799312 | 89.9% |
Reaction Steps
3-((E)-2-Ethoxycarbonylvinyl)azetidine-1-carboxylic acid tert-butyl ester (0.95 g; 3.72 mmol) was dissolved in 1,4-dioxane (15 mL). Lithium hydroxide (0.098 g; 4.1 mmol) and water (10 mL) were added. The reaction mixture was stirred for 12 hours at room temperature. Water (70 mL) was added and the reaction mixture was washed with tert-butyl methyl ether (70 mL) and the phases were separated. The aqueous phase was adjusted to pH 2 with an aqueous solution of sodium hydrogensulfate (10%) and extracted with tert-butyl methylether (3×70 mL). The combined organic phases were dried (magnesium sulfate) and the solvent evaporated in vacuo to afford 0.76 g of 3-((E)-2-carboxyvinyl)azetidine-1-carboxylic acid tert-butyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06555570B2 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-ab8a700df1c045d0a9670e18e134db7c |
| Source note | uspto-grants-2003_04 |