Triethylamine → 3-Tert-butylphenyl methanesulfonate

HRID 1037704

반응식

HRID 1037704 반응식
[C:1]([C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>C1(C)C=CC=CC=1.O>[CH3:19][S:20]([O:11][C:7]1[CH:8]=[CH:9][CH:10]=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH:6]=1)(=[O:22])=[O:21]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 11450Phenol, 3-(1,1-dimethylethyl)-2회HCID 31297Methanesulfonyl chloride

생성물 1

HCID 594641483-Tert-butylphenyl methanesulfonate수율 88%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

반응 조건

온도
25 °C

실험 절차

8.00 g (53.3 mol) of 3-tert-butylphenol and 5.93 g (58.6 mol) of triethylamine were dissolved in 80 mL of toluene followed by dropping in 6.71 g (58.6 mol) of methanesulfonyl chloride over the course of 10 minutes at 10° C. followed by stirring for 10 minutes at 25° C. and confirming the 3-tert-butylphenol to no longer be present by gas chromatography. The reaction liquid was placed in water and following separation of the organic layer, was washed three times with water, once with saturated aqueous NaHCO3 solution and once with saturated brine followed by drying with MgSO4, concentrating and purifying the resulting residue by vacuum distillation to obtain 10.7 g (yield: 88%) of 3-tert-butylphenyl methanesulfonate.

후처리

  1. customThe reaction liquid
  2. customseparation of the organic layer
  3. washwas washed three times with water
  4. dry with materialby drying with MgSO4
  5. concentrationconcentrating
  6. custompurifying the resulting residue
  7. distillationby vacuum distillation

출처 및 근거

ORD 기록
ord-4fe6647686ae495087c803913e58b2fd
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546599B2

연결된 노트

불러오는 중…