Sec-Butylbenzene → 4-(Butan-2-yl)benzene-1-sulfonyl chloride

HRID 1925701노트

반응식

HRID 1925701 반응식
[CH:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([CH2:3][CH3:4])[CH3:2].P(Cl)(Cl)(Cl)(Cl)Cl.[Cl:17][S:18](O)(=[O:20])=[O:19]>ClCCCl>[CH:1]([C:5]1[CH:10]=[CH:9][C:8]([S:18]([Cl:17])(=[O:20])=[O:19])=[CH:7][CH:6]=1)([CH2:3][CH3:4])[CH3:2]

참가 물질

5

반응물 3

HCID 8680Sec-ButylbenzeneHCID 24638Chlorosulfonic acidHCID 24819Phosphorus pentachloride

생성물 1

HCID 37760484-(Butan-2-yl)benzene-1-sulfonyl chloride

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

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온도
80 °C

실험 절차

To a solution of commercially available sec-butylbenzene (1.34 g; 10 mmol) in 1,2-dichloroethane (50 mL) was added phosphorus pentachloride (2.5 g; 12 mmol) followed by chlorosulfonic acid (1.3 mL; 20 mmol) slowly. The mixture was heated at 80° C. overnight, then cooled to room temperature and mixed with ice water (150 mL). The organic phase was separated, and the aqueous phase was extracted with dichloromethane (2×10 mL). The organic phases were combined and dried over magnesium sulfate and concentrated under reduced pressure to give an orange oil which was used without further purification (2.3 g).

후처리

  1. temperaturecooled to room temperature
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with dichloromethane (2×10 mL)
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give an orange oil which
  7. customwas used without further purification (2.3 g)

출처 및 근거

ORD 기록
ord-b8e394d90157493fba6a2bb1d270ca01
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178699B2

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