Cyclopropylamine → HCID 771127、化合物

HRID 1449393ノート

反応式

HRID 1449393 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[CH:5]=[CH:6][C:7](Cl)=[O:8].[CH:13]1([NH2:16])[CH2:15][CH2:14]1>C1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7]([NH:16][CH:13]1[CH2:15][CH2:14]1)=[O:8]

参加物

4

反応物 2

HCID 69828CyclopropylamineHCID 53411290HCID 53411290、化合物

生成物 1

HCID 771127HCID 771127、化合物収率 75.6%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 3-chlorocinnamoyl chloride (6 g) in dry tolune (100 ml) was added with stirring to a solution of cyclopropylamine (6 g) in dry benzene (50 ml). The reaction mixture was allowed to stand at room temperature overnight, and the solvent was evaporated under reduced pressure. The residue was thoroughly triturated with water containing a small amount of sodium carbonate, washed with water and filtered. Recrystallization of the resulting crude product from ethanol-water (1:10) gave trans 3-chloro-N-cyclopropylcinnamamide (5 g), m.p. 112°-113° C. Elemented analysis, nmr and ir data were all consistent with the assigned structure. TLC gave one spot run on silica gel with 5:1 and with 3:1 hexane:ethanol.

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. customThe residue was thoroughly triturated with water containing a small amount of sodium carbonate
  3. washwashed with water
  4. filtrationfiltered
  5. customRecrystallization of the resulting crude product from ethanol-water (1:10)

出典と根拠

ORDレコード
ord-c3dc7821fa6a4f168a0ab82019f9f984
出典データセット
uspto-grants-1980_02
特許番号
US04190674

反応ノート

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