Triethylamine → 3,5-Di-tert-butylphenyl ethanesulfonate

HRID 1037703

반응식

HRID 1037703 반응식
[C:1]([C:5]1[CH:6]=[C:7]([OH:15])[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[CH2:23]([S:25](Cl)(=[O:27])=[O:26])[CH3:24]>C1(C)C=CC=CC=1>[CH2:23]([S:25]([O:15][C:7]1[CH:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=1)(=[O:27])=[O:26])[CH3:24]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11667Ethanesulfonyl chlorideHCID 708253,5-Di-tert-butylphenol2회

생성물 1

HCID 866395033,5-Di-tert-butylphenyl ethanesulfonate수율 91.3%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
25 °C

실험 절차

2.50 g (0.012 mol) of 3,5-di-tert-butylphenol and 1.27 g (0.013 mol) of triethylamine were dissolved in 15 mL of toluene followed by dropping in 1.62 g (0.013 mol) of ethanesulfonyl chloride over the course of 10 minutes at 5° C. Following completion of dropping, the mixture was stirred for 2 hours at 25° C. and the 3,5-di-tert-butylphenol was confirmed to no longer be present. The reaction liquid was placed in ice water and following separation of the organic layer, was washed twice with saturated brine followed by drying with MgSO4 and concentrating to obtain 3.27 g (yield: 91%) of 3,5-di-tert-butylphenyl ethanesulfonate. A purified product crystallized with n-hexane (white crystals, melting point: 52° C.) was used in a battery test.

후처리

  1. customThe reaction liquid
  2. customseparation of the organic layer
  3. washwas washed twice with saturated brine
  4. dry with materialby drying with MgSO4
  5. concentrationconcentrating

출처 및 근거

ORD 기록
ord-fe98c886bdab41f09ffa4b4644d7af53
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546599B2

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