Methyl iodide → HCID 19795770、化合物

Into 50 ml of acetonitrile were suspended 5.39 g (20.3 mmol), of 6-bromo-5-chlorovanillin, and 3.04 ml (20.3 mmol) of 1.8-diazabicyclo[5,4,0]-7-undecene and 2.53 ml (40.6 mmol) of methyl iodide were added dropwise under cooling with ice. After stirred for 5 hours at room temperature, 3.9 ml (22.33 mmol) if diisopropylethylamine and 2.53 ml (40.6 mmol) of methyl iodide were added under cooling with ice and the mixture was stirred for 20 hours at room temperature. After distilled off the solvent, 200 ml of dichloromethane were added to the residue, which was washed with water. After dried over anhydrous magnesium sulfate, the concentrated residue was purified by means of silica gel column chromatography (hexane-AcOEt 5:1) to obtain 4.04 g (yield 71%) of title compound as colorless needle-like crystals.

1. temperatureunder cooling with ice
2. temperatureunder cooling with ice
3. stirringthe mixture was stirred for 20 hours at room temperature
4. distillationAfter distilled off the solvent, 200 ml of dichloromethane
5. additionwere added to the residue, which
6. washwas washed with water
7. dry with materialAfter dried over anhydrous magnesium sulfate
8. customthe concentrated residue was purified by means of silica gel column chromatography (hexane-AcOEt 5:1)

ORDレコード

ord-c84f1c46a858498aa1a36a9d1af38093

出典データセット

uspto-grants-1993_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05244892