반응 #63155
ord-cad2be3f15de4c6eaa93a331efc5ead5
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONwas added portionwise at a rate
- 2온도to maintain a reflux temperature of about 130°-135° C
- 3온도The mixture was refluxed an additional two hours
- 4여과filtered
- 5농축the filtrate was concentrated in vacuo
실험 절차
A suspension of 8 g of the product of Example 7 and 0.4 g of DABCO in 90 ml of xylenes was heated under N2 at 130°-135° C. while 1.8 ml of phosgene was added portionwise at a rate to maintain a reflux temperature of about 130°-135° C. The mixture was refluxed an additional two hours, cooled under N2 to room temperature, filtered, and the filtrate was concentrated in vacuo to yield 6.9 g of the subject compound as a crude oil.