Hexane → HCID 13124064、化合物

Hexane (1 ml) was added to (cyclopentadienyl)(1-[(1'S,2'S,5'R)-2'-isopropyl-5'-methylcyclohexyl]-4,5,6,7-tetrahydroindenyl)zirconium dichloride complex (20 mg, 4 mol %, prepared as in Example 1) in a 25 ml schlenk flask containing a stirring bar. Allylphenylthioether (150 mg, 1 mmol) was added and the flask evacuated and refilled 3 times with argon. Triethylaluminum (6 ml, 1.0 M in hexane, 6 mmol, 6 eq) was added dropwise. The solution turned yellow and was left for 72 hours. Water (10 ml) was added dropwise, the organics were extracted with diethylether (3×5 ml) and the combined extracts were dried over magnesium sulphate. The solvents were removed under reduced pressure and Kugelrohr distillation yielded the title compound as a clear liquid (145 mg, 0.85 mmnol, 80.5% yield, e.e 57% (FS-Hydrodex-B, 110° C.)).

1. additioncontaining a stirring bar
2. customthe flask evacuated
3. additionrefilled 3 times with argon
4. extractionthe organics were extracted with diethylether (3×5 ml)
5. dry with materialthe combined extracts were dried over magnesium sulphate
6. customThe solvents were removed under reduced pressure and Kugelrohr distillation

ORDレコード

ord-b6547e5b490a4b918955451e374db46a

出典データセット

uspto-grants-1999_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05929266