HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 89431891, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| Reactant | HCID 87306933 | HCID 87306933 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 89431891 | HCID 89431891 | 44% |
Reaction Conditions
| Temperature | 220 °C |
|---|
Reaction Steps
To a solution of Example 75 (50 mg, 0.13 mmol) in NMP (2 mL) was added methylamine hydrochloride (18 mg, 0.26 mmol) and DIPEA (0.5 mL). The mixture was heated in a microwave at 220° C. for 2 h. Purification by preparative HPLC (Method 1) gave the title compound as an off-white solid (23 mg, 44%). δH (CDCl3) 8.17 (s, 1H), 7.63-7.70 (m, 3H), 7.38-7.57 (m, 5H), 5.47 (s, 1H), 4.80-4.95 (m, 2H), 4.69 (d, J 5.8 Hz, 2H), 2.91 (d, J 5.1 Hz, 3H), 2.81 (s, 3H), 2.14 (s, 3H). LCMS (ES+) 370.2 (M+H)+, RT 2.34 minutes (Method 3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399483B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-29b3e9d4fea540699ae33deb51026d22 |
| Source note | uspto-grants-2013_03 |