반응 #529722
ord-3588129e77b44388bd27bcd1bd61138c
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반응 조건
후처리
- 1workup.ADDITIONtreated with 204 g
- 2workup.ADDITIONtreated dropwise with 500 ml
- 3workup.ADDITIONAfter addition
- 4workup.ADDITIONat -70° C. treated with 182 g
- 5workup.WAITto come to room temperature overnight
- 6세척The methylene chloride solution was washed twice with 3 liters of ice water
- 7건조by drying over sodium sulfate
- 8농축concentrating the dried solution to a yellow oil under reduced pressure
- 9workup.ADDITIONtreated with 1 liter of 1N hydrochloric acid
- 10온도refluxed for 2 hrs
- 11온도After cooling in an ice bath 343 g
- 12기타(79.9%) of crude produce
- 13기타was recovered
- 14여과after filtering
- 15기타drying
- 16기타Two recrystallizations from toluene
- 17기타gave creamy white flakes
실험 절차
A solution of 300 g. (1.52 mole) of 2-aminobenzophenone in 4 liters of methylene chloride was chilled to -40° C. and then treated with 204 g. (1.52 mole) of the ethyl α-(methylthio)acetate dissolved in 5 liters of methylene chloride. The reaction mixture was then cooled to -65° C. and treated dropwise with 500 ml. of a methylene chloride solution containing 164 g. (1.52 mole) of t-butylhypochlorite. After addition was complete, stirring was continued for 2 hr. at -70° C. treated with 182 g. (1.8 mole) of triethylamine and allowed to come to room temperature overnight. The methylene chloride solution was washed twice with 3 liters of ice water followed by drying over sodium sulfate and concentrating the dried solution to a yellow oil under reduced pressure. The oil was taken into 1.5 liters of methanol treated with 1 liter of 1N hydrochloric acid and refluxed for 2 hrs. After cooling in an ice bath 343 g. (79.9%) of crude produce was recovered after filtering and drying. Two recrystallizations from toluene gave creamy white flakes; m.p. 130° C.