Potassium thiocyanate → 4-methyl-N-(2,2,2-trifluoro-1-isothiocyanatoethyl)benzamide

HRID 479472ノート

反応式

HRID 479472 の反応式
Cl[CH:2]([NH:7][C:8](=[O:16])[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)[C:3]([F:6])([F:5])[F:4].[S-:17][C:18]#[N:19].[K+]>CC(C)=O>[CH3:15][C:12]1[CH:13]=[CH:14][C:9]([C:8]([NH:7][CH:2]([N:19]=[C:18]=[S:17])[C:3]([F:6])([F:5])[F:4])=[O:16])=[CH:10][CH:11]=1

参加物

4

反応物 2

HCID 516872Potassium thiocyanateHCID 12150323N-(1-chloro-2,2,2-trifluoroethyl)-4-methylbenzamide

生成物 1

HCID 121503244-methyl-N-(2,2,2-trifluoro-1-isothiocyanatoethyl)benzamide収率 61.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A stirred solution of Example 1B (2.00 g, 8.00 mmol) in acetone (35 mL) at ambient temperature was treated with potassium thiocyanate (1.60 g, 16.0 mmol). The reaction mixture was stirred for 12 hours, concentrated, and the crude residue was purified by flash chromatography (elution with 40% ethyl acetate/hexanes) to provide 1.34 g of the desired product as an off-white solid.

後処理

  1. concentrationconcentrated
  2. customthe crude residue was purified by flash chromatography (elution with 40% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-ae1143b2e1d6485fa6570a5ad5d8b773
出典データセット
uspto-grants-2003_11
特許番号
US06645968B2

反応ノート

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