海萝胶 → 3-溴苯甲醇

Into a solution of 370 g. of 3-bromo benzaldehyde, 900 cm3. of methanol and 300 g. of 40% formaldehyde the solution of 380 g. of potassium hydroxide in 300 cm3. of water are dropped at a temperature of from 48° to 52° C. during 10 minutes while stirring. The reaction mixture is stirred for 3.5 hours at a temperature of from 50° to 55° C. Into this reaction mixture the solution of 60 g. of potassium hydroxide in 40 cm3. of water are dropped at 55° C. then the reaction mixture is stirred at 60° C. for 1.5 hours. After cooling to ambient temperature the pH-value of the reaction mixture is adjusted with 250 cm3. of an aqueous hydrochloric acid solution /1:1/ to 9. From this reaction mixture the methanol is distilled off, 2 l. of water are added to the residue and twice extracted with 400 cm3. of 1,2-dichloro ethane. After distilling the dichloro ethane off the residue is fractionated in vacuo. 333 g. of 3-bromobenzyl alcohol are obtained. Boiling point 120°-122° C./266-399 Pa.

1. stirringThe reaction mixture is stirred for 3.5 hours at a temperature of from 50° to 55° C
2. stirringthe reaction mixture is stirred at 60° C. for 1.5 hours
3. distillationFrom this reaction mixture the methanol is distilled off
4. additionof water are added to the residue
5. extractiontwice extracted with 400 cm3
6. distillationAfter distilling the dichloro ethane off the residue

ORD记录

ord-24311de4fcac418c8b2f6d011a5f0ad3

来源数据集

uspto-grants-1987_11

DOI

10.6084/m9.figshare.5104873.v1

专利号

US04709081