Chlorosulfonic acid → 5,5,8,8-Tetramethyl-5,6,7,8-tetrahydro-2-naphthalenesulfonyl chloride

HRID 6508

反応式

HRID 6508 の反応式
[CH3:1][C:2]1([CH3:14])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([CH3:13])([CH3:12])[CH2:4][CH2:3]1.[Cl:15][S:16](O)(=[O:18])=[O:17]>>[CH3:1][C:2]1([CH3:14])[CH2:3][CH2:4][C:5]([CH3:13])([CH3:12])[C:6]2[CH:7]=[C:8]([S:16]([Cl:15])(=[O:18])=[O:17])[CH:9]=[CH:10][C:11]1=2

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 811861,1,4,4-Tetramethyltetralin

生成物 1

HCID 27954675,5,8,8-Tetramethyl-5,6,7,8-tetrahydro-2-naphthalenesulfonyl chloride

反応条件

温度
60 °C

実験手順

94.0 g (0.5 mol) of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene were stirred into 100 ml of chlorosulfonic acid at 20° C. within 30 min. The reaction solution was maintained at 60° C. for 1 hour, cooled to room temperature and then poured into 1.5 l of ice and extracted with ether. The organic phase was washed to neutrality with brine and water, dried over magnesium sulfate and evaporated under reduced pressure. Recrystallization of the residue from methanol yielded 55.0 g of 5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-sulfonyl chloride of melting point 71°-74° C.

後処理

  1. temperaturecooled to room temperature
  2. extractionextracted with ether
  3. washThe organic phase was washed
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customRecrystallization of the residue from methanol

出典と根拠

ORDレコード
ord-870f165d08ed449088d95aa4882d0671
出典データセット
uspto-grants-1993_09
特許番号
US05248823

関連ノート

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