Lawesson's reagent → Tert-butyl Dithiobenzoate

HRID 1445972ノート

反応式

HRID 1445972 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 9920756Tert-butyl Dithiobenzoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-b89bcb5ea99f43fbb13832dc70539f66
出典データセット
uspto-grants-2010_02
特許番号
US07666962B2

反応ノート

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