HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → (S)-[4-(2-Amino-pyridin-3-ylmethyl)-7-cyano-1,2,3,4-tetrahydro-cyclopenta[b]indol-2-yl]-carbamic acid isopropyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | (S)-{7-cyano-4-[2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-pyridin-3-ylmethyl]-1,2,3,4-tetrahydro-cyclopenta[b]indol-2-yl}-carbamic acid isopropyl ester | HCID 59242747 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (S)-[4-(2-Amino-pyridin-3-ylmethyl)-7-cyano-1,2,3,4-tetrahydro-cyclopenta[b]indol-2-yl]-carbamic acid isopropyl ester | HCID 24963751 | 13.3% |
Reaction Steps
Combine crude (S)-{7-cyano-4-[2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-pyridin-3-ylmethyl]-1,2,3,4-tetrahydro-cyclopenta[b]indol-2-yl}-carbamic acid isopropyl ester (2.12 mmol, 1100 mg crude material) in a mixture of THF (22 mL) and ethanol (4 mL) and stir for 15 min. Add hydrazine hydrate 0.5 mL, 10 mmol) and stir the mixture at room temperature for 18 h. Vacuum filter the crude reaction and wash the solid with THF (50 mL). Collect the filtrate and remove the solvent under vacuum. Purify the resulting residue by silica gel chromatography (50-100% ethyl acetate/CH2Cl2) to provide 110 mg (13%) of the title compound. MS (m/z): 390 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968587B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-a7da92ad101041b19ee5fb70af62631f |
| Source note | uspto-grants-2011_06 |