Triethylamine → 3-Tert-butylphenyl methanesulfonate

HRID 1037704ノート

反応式

HRID 1037704 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 594641483-Tert-butylphenyl methanesulfonate収率 88%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4fe6647686ae495087c803913e58b2fd
出典データセット
uspto-grants-2013_10
特許番号
US08546599B2

反応ノート

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