Hydrochloric Acid → HCID 13042967, 화합물

To a stirred solution of the epoxide (177 mg, 1 mmol, Example 303) in tetrahydrofuran (8 mL), lithium bromide (543 mg, 6.25 mmol, Aldrich) and copper(II)bromide (725 mg, 3.25 mmol, Aldrich) were added and the mixture was stirred at room temperature overnight. The mixture was poured into 0.1N hydrochloric acid (33 mL) and extracted with ethyl acetate (3×10 mL). The extracts were combined, washed with water, brine and dried with MgSO4. The solvent was removed to give the desired product as colorless oil after passing through an aluminum column (eluted with 5% methanol/dichloromethane). 237 mg, 92%. H1NMR (300 MHz, CDCl3), ppm: 2.00-2.20 (m), 1 H; 2.38-2.52 (m), 1 H; 2.70 (br), 1 H (OH); 2.99 (s), 3H; 3.0-3.20 (m), 2 H; 3.50-3.51 (m), 1 H; 3.80-3.97 (m), 2 H; 4.0-4.10 (m), 1 H. The compound was used directly for the next step.

1. extractionextracted with ethyl acetate (3×10 mL)
2. washwashed with water, brine
3. dry with materialdried with MgSO4
4. customThe solvent was removed

ORD 기록

ord-02ff125a184b4d17bc63c6dbef7a2fe6

출처 데이터셋

uspto-grants-2009_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07615634B2