HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropylamine → 2-Fluoro-6-iodo-3-[(isopropylamino)methyl]benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropylamine | HCID 6363 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 2-Fluoro-3-formyl-6-iodobenzonitrile | HCID 86019349 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2-Fluoro-6-iodo-3-[(isopropylamino)methyl]benzonitrile | HCID 66681152 | 32.5% |
Reaction Steps
A solution of Example 220A (1.00 g, 3.6 mmol) in MeOH (15 mL) was treated with isopropylamine (0.31 mL, 3.6 mmol) and sodium cyanoborohydride (227 mg, 3.6 mmol), and the mixture was stirred overnight at rt. HOAc (1 mL) was added and the reaction was stirred for 5 h, then treated with 1N NaOH and extracted with EtOAc. The extracts were washed with brine, dried (MgSO4) and concentrated. The residue was purified by flash chromatography on silica gel eluting with 8% MeOH/CH2Cl2 to give the desired product (372 mg). MS (ESI(+)) m/e 318.9 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07297709B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-4f211c8740bc42f0b904cf8b2d4a3b11 |
| Source note | uspto-grants-2007_11 |