Hydrochloric Acid → 1-Nitro-2-phenylethane

2-Phenylnitroethene (5.12 g, 34.3 mmol, from step 15a) was dissolved in CHCl3 /i-PrOH (410:85 mL) and SiO2 (51.4 g) was added. NaBH4 (5.2 g, 137 mmol) was added in portions, and the mixture was stirred for 90 minutes at room temperature. HCl (0.5N, 100, mL) was added, and the mixture was stirred for 30 minutes. The layers were separated, and the aqueous phase was extracted with methylene chloride. The organic layers were combine, dried (MgSO4) and concentrated. The residue was chromatographed on silica gel (eluting with ether:hexanes 1:30) to give the title compound as an oil (3.89 g, 75%).

1. stirringthe mixture was stirred for 30 minutes
2. customThe layers were separated
3. extractionthe aqueous phase was extracted with methylene chloride
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe residue was chromatographed on silica gel (eluting with ether:hexanes 1:30)

ORDレコード

ord-d656571e780d4bccad9fd6471b2c4bc3

出典データセット

uspto-grants-1998_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05733912