Pentane → HCID 123757656, compound

Temperature

70 °C

Diisobutylchlorosilane (18.0 mL, 100 mmol) was dissolved in THF (100 mL), and tert-butyl magnesium chloride THF solution (10M, 100 mL) was added dropwise thereto under nitrogen for 30 minutes. Cuprous bromide (286 mg, 2.00 mmol) was added to the resultant mixture, followed by stirring at 70° C. for 8 hours. The reaction mixture was left to cool, and saturated aqueous ammonium chloride and n-pentane were added thereto. The formed organic layer was washed three times with water and once with saturated brine, and the thus-washed layer was dried over sodium sulfate anhydrate. The solvent was removed, followed by purification through distillation under reduced pressure, whereby the Compound 36a was obtained as a colorless liquid (boiling point; 27 mmHg, 100° C. fraction, 13.6 g, 68%).

1. waitThe reaction mixture was left
2. temperatureto cool
3. washThe formed organic layer was washed three times with water
4. dry with materialonce with saturated brine, and the thus-washed layer was dried over sodium sulfate anhydrate
5. customThe solvent was removed
6. distillationfollowed by purification through distillation under reduced pressure, whereby the Compound 36a
7. customwas obtained as a colorless liquid (boiling point; 27 mmHg, 100° C. fraction, 13.6 g, 68%)

ORD record

ord-ec5fb26113ea454f83377c8a91b4bf8d

Source dataset

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07825103B2