Hexane → HCID 71307795、化合物

A solution of 5-methyloxazole (5.0 g, 60.2 mmol) in Et2O (100 mL) was cooled to −78° C. under N2 and treated with a 1.6 M solution of BuLi in hexane (41.4 mL, 66.2 mmol) dropwise. The mixture was stirred at −78° C. for 30 min and a solution of Bu3SnCl (16.31 mL, 60.2 mmol) in Et2O (50 mL) was then added dropwise. The mixture was stirred at −78° C. for another 30 min and then allowed to warm to RT. The reaction mixture was filtered on celite, and the filtrate concentrated in vacuo. Purification by distillation (0.1 Torr, 128-130° C.) afforded the title compound (3.5 g) as a yellow liquid. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 0.88 (m, 12 H) 1.14-1.22 (m, 6 H) 1.27-1.38 (m, 6 H) 1.52-1.61 (m, 6 H) 2.17-2.21 (m, 3 H) 7.49-7.54 (m, 1 H).

1. stirringThe mixture was stirred at −78° C. for another 30 min
2. temperatureto warm to RT
3. filtrationThe reaction mixture was filtered on celite
4. concentrationthe filtrate concentrated in vacuo
5. customPurification
6. distillationby distillation (0.1 Torr, 128-130° C.)

ORDレコード

ord-46bbe033228d47e5895f7fc9ce76a2f6

出典データセット

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08853203B2