Lawesson's reagent → HCID 58092092, 화합물

HRID 1873477

반응식

HRID 1873477 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 58092092HCID 58092092, 화합물수율 58.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

(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).

후처리

  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

출처 및 근거

ORD 기록
ord-53026bfe1290432799842ee53390aeaf
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304371B2

연결된 노트

불러오는 중…