Sodium Cyanate → 1-Isopropyl-1-(4-methoxy-phenyl)-urea

HRID 445150ノート

反応式

HRID 445150 の反応式
[CH:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[CH:7][CH:6]=1)([CH3:3])[CH3:2].[O-:13][C:14]#[N:15].[Na+]>C(O)(=O)C>[CH:1]([N:4]([C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[CH:7][CH:6]=1)[C:14]([NH2:15])=[O:13])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 517096Sodium CyanateHCID 27594984-methoxy-N-(propan-2-yl)aniline

生成物 1

HCID 130988041-Isopropyl-1-(4-methoxy-phenyl)-urea

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a solution of 4.47 g (27.1 mmol) isopropyl-(4-methoxy-phenyl)-amine in 70 ml acetic acid are added in small portions 1.72 g (25.4 mmol) sodium cyanate while keeping the temperature below 15° C. by means of an ice bath. After stirring for 2 h at room temperature the acetic acid is evaporated and the residue is taken up in dichloromethane and washed with aqueous sodium hydroxide solution (1M). The organic phase is evaporated and the crude product is purified by recrystallization from dichloromethane/hexanes to yield 1-isopropyl-1-(4-methoxy-phenyl)-urea.

後処理

  1. customthe temperature below 15° C.
  2. customis evaporated
  3. washwashed with aqueous sodium hydroxide solution (1M)
  4. customThe organic phase is evaporated
  5. customthe crude product is purified by recrystallization from dichloromethane/hexanes

出典と根拠

ORDレコード
ord-48fca9add93343c28be773acf4447825
出典データセット
uspto-grants-2013_07
特許番号
US08476286B2

反応ノート

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