Lawesson's reagent → Tert-butyl Dithiobenzoate

HRID 2236048노트

반응식

HRID 2236048 반응식
[C:1]([S:9][C:10]([CH3:13])([CH3:12])[CH3:11])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1>C1(C)C=CC=CC=1>[C:1]([S:9][C:10]([CH3:13])([CH3:12])[CH3:11])(=[S:23])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 12492106S-tert-Butyl benzenecarbothioate

생성물 1

HCID 9920756Tert-butyl Dithiobenzoate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of S-t-butyl thiobenzoate (1.94 g, 0.01 mol) and Lawesson's reagent (2.43 g, 0.006 mol) in anhydrous toluene (10 mL) was refluxed for 25 hours. After cooling to room temperature, the reaction mixture was concentrated and the residue subjected to column chromatography (Kieselgel-60, 70-230 mesh, petroleum spirit/diethyl ether 19:1) The title compound was obtained as an oil, 1.37 g (65.5%). 1H-nmr (CDCl3) d (ppm): 1.69 (s, 9H, 3×CH3), 7.36 (m, 2H, meta-ArH), 7.50 (m, 1H, para-ArH) and 7.88 (d, 2H, ortho-ArH).

후처리

  1. temperaturewas refluxed for 25 hours
  2. concentrationthe reaction mixture was concentrated
  3. customwas obtained as an oil, 1.37 g (65.5%)

출처 및 근거

ORD 기록
ord-2e842d6d7d9148cc9bb6f890d20d54f6
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07714075B1

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