HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59496620, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 3-Amino-3-cyclohexylpropanoic acid | HCID 2733681 | — |
| Product | HCID 59496620 | HCID 59496620 | 97.1% |
Reaction Steps
Methyl chloroformate (54 uL, 0.70 mmol) was added to a mixture of 3-amino-3-cyclohexylpropanoic acid (100.0 mg, 0.5840 mmol) (Key Organics/Bionet, Cat. #7T-0112) and potassium carbonate (160 mg, 1.2 mmol) in water (2.0 mL, 110 mmol) and tetrahydrofuran (2.0 mL, 25 mmol). After stirring at r.t. for 10 min, the mixture was extracted with ether to remove impurity. The aqueous layer was adjusted to pH=2 with HCl, and extracted with ethyl acetate (3×10 mL). The combined organic layers were dried over MgSO4, filtered and concentrated under reduced pressure to afford the desired product (130 mg, 97%). Analytic LCMS (M+H)+: m/z=230.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481732B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-bc634a5758574bf798c8210d5c416cda |
| Source note | uspto-grants-2013_07 |