Lawesson's reagent → HCID 58092092、化合物

HRID 1873477

反応式

HRID 1873477 の反応式
[C:1]([O:4][CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([C:16](=O)[NH:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])=[CH:8][CH:7]=1)(=[O:3])[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:33])=CC=1>C1(C)C=CC=CC=1>[C:1]([O:4][CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([C:16](=[S:33])[NH:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])=[CH:8][CH:7]=1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 58092097(4{[(Trimethylsilyl)methyl]carbamoyl}naphthalen-1-yl)methyl acetate

生成物 1

HCID 58092092HCID 58092092、化合物収率 58.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

(4{[(trimethylsilyl)methyl]carbamoyl}naphthalen-1-yl)methyl acetate (2.0 g) and Lawesson reagent (2.4 g) were suspended with toluene (30 ml). The mixture was heated to reflux for 2 hours. The reaction mixture was returned to room temperature, washed with water and a saturated aqueous brine, subsequently dried over magnesium sulfate. After filtering the reaction mixture, the solvent was distilled off under reduced pressure, and the resulting mixture was purified by silica gel chromatography, to obtain (4{[(trimethylsilyl)methyl]carbamothioyl}naphthalen-1-yl)methyl acetate (1.2 g).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 2 hours
  3. customwas returned to room temperature
  4. washwashed with water
  5. dry with materiala saturated aqueous brine, subsequently dried over magnesium sulfate
  6. filtrationAfter filtering the reaction mixture
  7. distillationthe solvent was distilled off under reduced pressure
  8. customthe resulting mixture was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-53026bfe1290432799842ee53390aeaf
出典データセット
uspto-grants-2012_11
特許番号
US08304371B2

関連ノート

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