Trichlorosilane → HCID 88546075, compound

In a heavy-walled tube equipped with a magnetic stir bar, ester (19) (3.97 g, 20.0 mmol, 1.0 equiv.) and H2PtCl6.6H2O (104 mg, 0.20 mmol, 1.0 mol. %) were loaded. The tube was transferred into a glovebox and HSiCl3 (4.10 mL, 40.2 mmol, 2.0 equiv.) was added to the solution. The tube was tightly fastened then removed from the glovebox. The resulting solution was stirred at room temperature for 20 h behind a protecting shield. Purification was achieved by Kugelrohr distillation under high vacuum and provided 5.46 g (82%) of 7-OEG (20) as a colourless oil; bp=115-120° C. (0.09 Torr); 1H NMR (400 MHz, CDCl3) δ 4.52 (m, 2H), 3.76 (m, 2H), 3.56 (t, J=6.2 Hz, 2H), 1.85 (m, 2H), 1.48 (m, 2H); 13C NMR (100 MHz, CDCl3) δ 157.7 (q, J=42.3 Hz), 114.7 (q, J=284.1 Hz), 71.8, 67.9, 67.0, 22.8, 21.0.

1. customIn a heavy-walled tube equipped with a magnetic stir bar
2. customThe tube was transferred into a glovebox
3. customThe tube was tightly fastened then removed from the glovebox
4. customPurification
5. distillationwas achieved by Kugelrohr distillation under high vacuum

ORD record

ord-952577db74594e4cb704d18c40e54c52

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08491958B2