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

HRID 1037703

反応式

HRID 1037703 の反応式
[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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11667Ethanesulfonyl chlorideHCID 708253,5-Di-tert-butylphenol2 回

生成物 1

HCID 866395033,5-Di-tert-butylphenyl ethanesulfonate収率 91.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fe98c886bdab41f09ffa4b4644d7af53
出典データセット
uspto-grants-2013_10
特許番号
US08546599B2

関連ノート

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