Lawesson's reagent → Benzenecarbothioamide, 4-bromo-3-methyl-

HRID 1741051ノート

反応式

HRID 1741051 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=O)=[CH:4][C:3]=1[CH3:11].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:21])=CC=1>C1COCC1>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[S:21])=[CH:4][C:3]=1[CH3:11]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 70208694-bromo-3-methylbenzamide

生成物 1

HCID 21833829Benzenecarbothioamide, 4-bromo-3-methyl-収率 157.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4-Bromo-3-methylbenzamide (D37, 1.0 g, 0.0047 mole) was dissolved in THF (50 ml), treated with Lawessons reagent (0.95 g, 0.0024 mole) and stirred under argon for 4 h. The solvent was removed in vacuo and the residue purified by flash chromatography on silica gel eluting with 10% EtOH/CHCl3 to afford the title compound as a yellow solid (0.87 g, 80%).

後処理

  1. customThe solvent was removed in vacuo
  2. customthe residue purified by flash chromatography on silica gel eluting with 10% EtOH/CHCl3

出典と根拠

ORDレコード
ord-8110713d4b2a4452b5d593091695d896
出典データセット
uspto-grants-1999_10
特許番号
US05972951

反応ノート

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