Imidazole → HCID 21180673、化合物

A solution of 2.00 g (11.6 mmol) of 3-(3,4difluorophenyl)propanol (from EXAMPLE 199, Step A), 3.96 g (15.1 mmol) of triphenylphosphine and 1.03 g (15.1 mmol) of imidazole in 2:1 v/v ether/CH3CN at 0° C. was treated with 4.10 g (16.3 mmol) of iodine. The resulting mixture was warmed to rt and stirred for 1 h. The mixture was diluted with 200 mL ether, and washed with sat'd Na2S2O3 (2×30 mL) and sat'd CuSO4 (30 mL). The organic phase was dried over MgSO4 and concentrated. The residue was partially dissolved in ether and filtered to remove triphenylphosphine oxide. The filtrate was concentrated. Flash chromatography on silica gel using 4:1 v/v hexanes/EtOAc afforded 3.25 g (99%) of the title compound.

1. washwashed with sat'd Na2S2O3 (2×30 mL) and sat'd CuSO4 (30 mL)
2. dry with materialThe organic phase was dried over MgSO4
3. concentrationconcentrated
4. dissolutionThe residue was partially dissolved in ether
5. filtrationfiltered
6. customto remove triphenylphosphine oxide
7. concentrationThe filtrate was concentrated

ORDレコード

ord-a500c7d5fbb4460ebf6e1ccd11c1a3ae

出典データセット

uspto-grants-2001_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06265434B1