Benzene → 4-Benzyloxybenzyl chloride

In a 1 l four-necked flask, there were placed 85.4 g (0.464 mole) of benzyl phenyl ether, 45 g (1.5 moles) of paraformaldehyde, 300 ml of conc. hydrochloric acid and 100 ml of benzene, and the resulting mixture was stirred for 4 hours at 50° to 60° C. After completion of the reaction, 100 ml of toluene was added to the resulting reaction mixture followed by vigorous stirring of the resulting mixture. The resulting organic layer in the mixture was washed twice with 200 ml of water. The thus obtained organic layer was dried over anhydrous sodium sulfate followed by removal of the solvent by evaporation. To the so obtained viscous oily substance were added about 200 ml of n-heptane and 50 ml of ethyl ether. Upon stirring of the resulting mixture at room temperature, crystals precipitated. After allowing the mixture to stand overnight, the crystals were collected by filtration and dried to give 30.5 of 4-benzyloxybenzyl chloride.

1. customIn a 1 l four-necked flask, there were placed
2. additionwas added to the resulting reaction mixture
3. washThe resulting organic layer in the mixture was washed twice with 200 ml of water
4. dry with materialThe thus obtained organic layer was dried over anhydrous sodium sulfate
5. customfollowed by removal of the solvent by evaporation
6. additionTo the so obtained viscous oily substance were added about 200 ml of n-heptane and 50 ml of ethyl ether
7. stirringUpon stirring of the resulting mixture at room temperature
8. customcrystals precipitated
9. filtrationthe crystals were collected by filtration
10. customdried

ORDレコード

ord-c0c49502049f43029eb6bdb3f1fbb24a

出典データセット

uspto-grants-1983_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04412082