تفاعل #8505
ord-4caad36be5ac4269aa3917d91c05067e
معادلة التفاعل
ظروف التفاعل
درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe reaction mixture was cooled down
- 2أخرىseparated
- 3workup.ADDITIONafter the addition of water (90 ml)
- 4workup.ADDITIONTo the organic layer was added sulfuric acidic brine
- 5أخرىseparated
- 6workup.ADDITIONmixed with ethyl acetate
- 7تركيزconcentrated under reduced pressure
الإجراء التجريبي
To 48% aqueous sodium hydroxide (127.8 g) was added tetra-n-butylammonium bromide (3.3 g, 10 mmol). The mixture was heated to 60° C. To the mixture was added 2-butene-1,4-diol (17) (30.0 g, 340 mmol), to which was added dropwise benzyl chloride (94.8 g, 743 mmol) at 80±15° C. The mixture was stirred at the same temperature for 2 hours. The reaction mixture was cooled down, and separated after the addition of water (90 ml). To the organic layer was added sulfuric acidic brine. The solution was neutralized by aqueous sodium hydrogen carbonate, separated, mixed with ethyl acetate and concentrated under reduced pressure to yield the objective (18) (104.5 g, quantitative) as an oil residue.