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

HRID 260585

반응식

HRID 260585 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

반응 조건

온도
60 °C

실험 절차

94.0 g (0.5 mol) of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene were stirred into 100 ml 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.

후처리

  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

출처 및 근거

ORD 기록
ord-b7bcb2cb8d2546dfa460c549201095bd
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527945

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