HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 69307287, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 69309708 | HCID 69309708 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69307287 | HCID 69307287 | — |
Reaction Steps
To DCM (8 mL) was added (4-benzotriazol-1-yl-pyrimidin-2-yl)-piperidin-3-ylamine (0.15 g), methanesulfonyl chloride (35 μL) and TEA (0.285 mL), and the mixture stirred at RT. The product was purified by column chromatography on silica, using 100% DCM to 15% MeOH/DCM, then recrystallized from EtOAc to provide (4-benzotriazol-1-yl-pyrimidin-2-yl)-(1-methanesulfonyl-piperidin-3-yl)-amine. Mp=196.0-197.0° C., 1H nmr (300 MHz, DMSO-d6): δ ppm 1.40-1.76 (m, 2H), 1.78-2.14 (m, 2H), 2.72-2.86 (m, 2H), 2.89 (s, 3H), 3.49 (m, 1H), 3.78 (m, 1H), 4.02 (m, 1H), 7.41 (d, J=5.27 Hz, 1H), 7.58 (t, J=7.35 Hz, 1H), 7.73 (m, 1H), 8.22 (d, J=8.29 Hz, 1H), 8.55 (d, J=5.27 Hz, 1H), 8.88 (d, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08962622B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-da80a1c2b5b141b89111f68d6d537539 |
| Source note | uspto-grants-2015_02 |