HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 136348441, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 136348442 | HCID 136348442 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 136348441 | HCID 136348441 | 86.5% |
Reaction Steps
To a flask was added 3-(4-(1-ethyl-7-methyl-3-(pyridin-2-yl)-4,6,7,8-tetrahydro-1H-pyrazolo[3,4-e][1,4]thiazepin-4-yl)-3-methylphenyl)prop-2-yn-1-ol (0.126 g, 0.301 mmol, prepared from P with Example #K.1 and prop-2-yn-1-ol), MeOH (7.53 ml) and THF (7.53 ml). The solution was treated with the H-Cube (Pd/C 10 wt %, Manual Control, 20 bar, 1 mL/min, rt) for about 2 h. The mixture was concentrated in vacuo and purified by flash chromatography (25 g silica gel; DCM/MeOH 1:0 to 9:1) to give 3-(4-(1-ethyl-7-methyl-3-(pyridin-2-yl)-4,6,7,8-tetrahydro-1H-pyrazolo[3,4-e][1,4]thiazepin-4-yl)-3-methylphenyl)propan-1-ol (0.110 g, 86%); LC-MS (Table 1, Method g) Rt=2.29 and 2.32 min.; MS m/z: 423.14 and 423.14 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150592B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-93b655815f494b00967465657c1e6309 |
| Source note | uspto-grants-2015_10 |