Sodium Thiosulfate → HCID 86650637、化合物

1-(Allyloxy)-2-methylpropan-2-ol (1.50 g, 11.5 mmol) was dissolved in DCM (50 mL) and cooled to 0° C. mCPBA (77% max, 9.94 g) was added. The suspension was stirred at 0° C. for 6.5 hr. and then saturated NaHCO3 solution (˜20 ml) and Na2S2O3 solution (˜20 ml) were added. The resulting mixture was stirred at 0° C. for 15 min and the two layers were separated. The aqueous layer was extracted twice with DCM. The organic layers were combined, dried over Na2SO4 and concentrated. The resulting residue was purified on a silica gel column (heptane:EtOAc 1:0 to 1:2) to give the product as a colorless oil (620 mg, 37%). 1H NMR (400 MHz, CDCl3) δ ppm 3.64 (1H, ddd, J=12.0, 5.2, 2.8 Hz), 3.24-3.29 (1H, m), 3.17-3.21 (1H, m), 3.11-3.14 (1H, m), 2.97-3.00 (1H, m), 2.88 (1H, br s), 2.60-2.64 (1H, m), 2.44-2.47 (1H, m), 1.02 (6H, s).

1. additionwas added
2. stirringThe resulting mixture was stirred at 0° C. for 15 min
3. customthe two layers were separated
4. extractionThe aqueous layer was extracted twice with DCM
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customThe resulting residue was purified on a silica gel column (heptane:EtOAc 1:0 to 1:2)

ORDレコード

ord-09e7d63b125c4be7a0bdd2410bb04934

出典データセット

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08778951B2