반응 #2487486

반응 방정식

4-Iodobenzoic acid

→

4-Iodobenzoic Acid tert-butyl Ester

용매

toluene

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONThe reaction was mixed for 16 h
2. 2
   온도cooled from 70° C. to rt
3. 3
   온도The solution was heated to 70° C. for and
4. 4
   workup.ADDITIONmixed for 5 h
5. 5
   농축The sample was concentrated under vacuum, and AcOEt (400 ml)
6. 6
   workup.ADDITIONwas added
7. 7
   세척The solution was then washed with 1:1 sat. NaHCO3/water (150 ml), and sat. NaHCO3, water and sat. NaCl (75 ml each)
8. 8
   건조The organic phase was dried (MgSO4)
9. 9
   농축concentrated under vacuum
10. 10
    기타to yield a light brown oil

실험 절차

4-Iodobenzoic acid (10 g, 40.3 mmol) was dissolved in dry toluene (100 ml, dried over mol. sieves). The solution was heated to 70° C. under a flow of nitrogen. A solution of N,N′-dimethylformamide di-tert-butyl acetal (24.6 g, 121 mmol) in toluene (25 ml) was added over ca. 30 min. The reaction was mixed for 16 h. At some point the heating unit failed, So the reaction cooled from 70° C. to rt. The solution was heated to 70° C. for and mixed for 5 h. The sample was concentrated under vacuum, and AcOEt (400 ml) was added. The solution was then washed with 1:1 sat. NaHCO3/water (150 ml), and sat. NaHCO3, water and sat. NaCl (75 ml each). The organic phase was dried (MgSO4) and concentrated under vacuum to yield a light brown oil.

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