Potassium cyanate → 4-methyl-N-(2,2,2-trichloro-1-isocyanatoethyl)benzamide

HRID 479496ノート

反応式

HRID 479496 の反応式
[CH3:1][C:2]1[CH:16]=[CH:15][C:5]([C:6]([NH:8][CH:9](Cl)[C:10]([Cl:13])([Cl:12])[Cl:11])=[O:7])=[CH:4][CH:3]=1.[O-:17][C:18]#[N:19].[K+]>CC(C)=O>[CH3:1][C:2]1[CH:16]=[CH:15][C:5]([C:6]([NH:8][CH:9]([N:19]=[C:18]=[O:17])[C:10]([Cl:13])([Cl:12])[Cl:11])=[O:7])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 11378442Potassium cyanateHCID 123415764-Methyl-N-(1,2,2,2-tetrachloroethyl)benzamide

生成物 1

HCID 187707404-methyl-N-(2,2,2-trichloro-1-isocyanatoethyl)benzamide収率 60.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A stirred solution of Example 37D (1.00 g, 3.32.00 mmol) in acetone (20 mL) at ambient temperature was treated with potassium cyanate (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 50% ethyl acetate/hexanes) to provide 620 mg 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 50% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-67496c04989840a9921184ec86f9958e
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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