Tetrabutylammonium Fluoride → 1068560-15-5

HRID 1516244노트

반응식

HRID 1516244 반응식
[F-:1].C([N+](CCCC)(CCCC)CCCC)CCC.[CH3:19][O:20][C:21](=[O:34])[C:22]([CH3:33])([CH3:32])[CH2:23]OS(C(F)(F)F)(=O)=O>C1COCC1>[CH3:19][O:20][C:21](=[O:34])[C:22]([CH3:33])([CH3:32])[CH2:23][F:1]

참가 물질

4

반응물 2

HCID 2724141Tetrabutylammonium FluorideHCID 574170981163707-68-3

생성물 1

HCID 597024501068560-15-5

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

27 mL of a 1 M solution of tetrabutylammonium fluoride in THF are added slowly and under ice cooling to a solution of 7.25 g (27.4 mmol) 2,2-dimethyl-3-trifluoromethanesulfonyloxy-propionic acid methyl ester in 150 mL of THF. The resulting solution is stirred 6 h at 0° C. and then 10 h at RT. The solvent is evaporated carefully and the residue partitioned between DCM and brine. The organic phase is washed with brine, dried with sodium sulfate and evaporated carefully. The brown oil is distilled in a Kugelrohr-oven (oven temperature 120 to 150° C.) to give the title compound as a colorless liquid.

후처리

  1. custom10 h
  2. customat RT
  3. customThe solvent is evaporated carefully
  4. customthe residue partitioned between DCM and brine
  5. washThe organic phase is washed with brine
  6. dry with materialdried with sodium sulfate
  7. customevaporated carefully
  8. distillationThe brown oil is distilled in a Kugelrohr-oven (oven temperature 120 to 150° C.)

출처 및 근거

ORD 기록
ord-e998713125af4447b88f90d29bdd2c6b
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08227462B2

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