1,3-Dibromopropane → 1-(3-Bromopropoxy)-2-fluorobenzene

To a solution of 2-fluorophenol (0.040 mL, 0.448 mmol) in acetonitrile (4 mL) was added 1,3-dibromopropane (0.450 mL, 4.43 mmol) followed by Cs2CO3 (0.232 g, 0.713 mmol). The reaction mixture was stirred for 24 h and then concentrated under vacuum. The resulting residue was treated with H2O (4 mL) and extracted with DCM (8 mL). The organic layer was dried through a phase separator and concentrated under vacuum. The residue was taken up in DMSO and purified by preparatory HPLC (without TFA) to give the title compound (0.0274 g, 26.2%). EI-MS Rt (2.24 min).

1. concentrationconcentrated under vacuum
2. additionThe resulting residue was treated with H2O (4 mL)
3. extractionextracted with DCM (8 mL)
4. customThe organic layer was dried through a phase separator
5. concentrationconcentrated under vacuum
6. custompurified by preparatory HPLC (without TFA)

ORDレコード

ord-75daea08891645c2b76ac5cb1a1e57d2

出典データセット

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08853404B2