Lawesson's reagent → 4-bromo-3-chloro-N-trimethylsilanylmethylthiobenzamide

HRID 241518

반응식

HRID 241518 반응식
[Br:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([NH:8][CH2:9][Si:10]([CH3:13])([CH3:12])[CH3:11])=O)=[CH:4][C:3]=1[Cl:16].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:26])=CC=1>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([NH:8][CH2:9][Si:10]([CH3:13])([CH3:12])[CH3:11])=[S:26])=[CH:4][C:3]=1[Cl:16]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 668366994-bromo-3-chloro-N-trimethylsilanylmethyl-benzamide

생성물 1

HCID 866857054-bromo-3-chloro-N-trimethylsilanylmethylthiobenzamide수율 123.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a suspension of 4-bromo-3-chloro-N-trimethylsilanylmethyl-benzamide (34.00 g, 106.0 mmol) in toluene (250 mL) was added Lawesson's reagent (30.45 g, 75.28 mmol) at room temperature. The mixture was heated at reflux for 1 h and cooled to ambient temperature. After adsorption of the reaction mixture on silica gel the solvents were distilled off in vacuum. The residue was purified by flash chromatography on silica gel to give the title compound (31.3 g, 88%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 1 h
  3. distillationAfter adsorption of the reaction mixture on silica gel the solvents were distilled off in vacuum
  4. customThe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-883e5b94a177452c808aa72155b27f5a
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653000B2

연결된 노트

불러오는 중…