HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 11632767, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 11647366 | HCID 11647366 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 11632767 | HCID 11632767 | 79% |
Reaction Steps
Methyl 3-((4-(6-chlorothieno[2,3-d]pyrimidin-4-ylamino)piperidin-1-yl)methyl)benzoate (127 mg, 0.3 mmol) was heated in a 25% MeOH—H2O solution at 90° C. for 3 h in the presence of LiOH—H2O (12.7 mg, 0.3 mmol). The solvent was removed under reduced pressure; the residue was dissolved in MeOH and filtered. The filtrate was evaporated to collect product in 79% yield (97 mg). 1H NMR (400 MHz, CD3OD) δ 8.27 (s, 1H), 7.92 (s, 1H), 7.85 (d, 1H), 7.50 (s, 1H), 7.42 (d, 1H), 7.33 (t, 1H), 4.11 (m, 1H), 3.59 (s, 2H), 2.98 (d, 2H), 2.20 (t, 2H), 2.00 (d, 2H), 1.68 (m, 2H); MS (ESI) m/z: Calculated for C19H20ClN4O2S, 403.1; Observed: 403.2 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07612078B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-06aea33258834f47998baf68a14c33c3 |
| Source note | uspto-grants-2009_11 |