反应详情

According to the procedure of Soto et al, Synthesis, 483 (1983), a solution of 5-bromo-1-naphthoyl chloride (10.7 g, 39.8 mmol) in dry toluene (30 mL) was added dropwise to a mixture of ethyl benzimidate hydrochloride (7.4 g, 39.8 mmol) and triethylamine (8.9 g, 12.2 mL, 87.6 mmol) in dry toluene (100 mL). The mixture was stirred for 18 hours at room temperature, then heated to 70° C. for 60 hours. The mixture was cooled to room temperature and the preciptated salt removed by filtration and washed with toluene. The filtrate was concentrated in vacuo to give a red oil which crystallized upon drying in vacuo (15.2 g, guant.). This material was of sufficient purity to be used in the subsequent reaction.

1. customAccording to the procedure of Soto et al, Synthesis, 483 (1983)
2. temperatureheated to 70° C. for 60 hours
3. temperatureThe mixture was cooled to room temperature
4. customthe preciptated salt removed by filtration
5. washwashed with toluene
6. concentrationThe filtrate was concentrated in vacuo
7. customto give a red oil which
8. customcrystallized
9. customupon drying in vacuo (15.2 g, guant.)
10. customto be used in the subsequent reaction