HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bis(trimethylsilyl)carbodiimide → HCID 178511903, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bis(trimethylsilyl)carbodiimide | HCID 70473 | — |
| Reactant | 6-Bromoflavanone | HCID 5270545 | — |
| Catalyst | Titanium Tetrachloride | HCID 24193 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178511903 | HCID 178511903 | 96% |
Reaction Steps
To a solution of 6-bromo-2-phenylchroman-4-one (387 mg, 1.28 mmol) in anhydrous DCM (10 mL) was added TiCl4 (1 M solution in DCM, 2.6 mL, 2.6 mmol) dropwise within 15 minutes at room temperature. The resulting mixture was stirred for 1 h after the addition. To this mixture was added bis-trimethylsilylcarbodiimide (525 mg, 2.82 mmol) dropwise. The resulting mixture was stirred for 18 h after the addition. The reaction mixture was poured into ice-water (50 g) and extracted with DCM (3×30 mL). The combined organic phases were dried over anhydrous Na2SO4, filtered, and concentrated to give (Z)—N-(6-bromo-2-phenylchroman-4-ylidene)cyanamide (400 mg, 96%) which was used in next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921359B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-dc33d890b8834059850548fedc75883d |
| Source note | uspto-grants-2014_12 |