HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 44125252, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 66873834 | HCID 66873834 | — |
| Product | HCID 44125252 | HCID 44125252 | 14.1% |
Reaction Steps
The title compound was synthesized from ethyl 5-methyl-1,4,5,6-tetrahydrocyclopenta[b]pyrrole-2-carboxylate (0.017 g, 0.09 mmol) and lithium hydroxide monohydrate (0.019 g, 0.45 mmol) according to General Procedure 7. The crude was purified by reverse phase HPLC (50-100% MeOH: water, 0.1% formic acid) to give 5-methyl-1,4,5,6-tetrahydrocyclopenta[b]pyrrole-2-carboxylic acid (22) as a light brown solid (2.1 mg, 14%). Rf (1:1 EtOAc:heptane)=0.12; 1H NMR (400 MHz, METHANOL-d4) δ ppm 1.19 (d, J=6.6, 3H), 2.17-2.20 (m, 1H), 2.26-2.32 (m, 1H), 2.75-2.80 (m, 1H), 2.84-2.90 (m, 2H), 6.56 (s, 1H); LCMS-MS (ESI+) 166.0 (M+H); HPLC (UV=100%), (ELSD=100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07902252B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-7422962b71f742be871699b368990add |
| Source note | uspto-grants-2011_03 |