Triethylamine → 2-[beta-(2-furyl)acrylamido]-N5-methyl-N1,N1-di(n-propyl)pentane-1,5-diamide

HRID 64925ノート

反応式

HRID 64925 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([OH:10])=O.C(N(CC)CC)C.C(Cl)(=O)OCC.Cl.[NH2:25][CH:26]([CH2:36][CH2:37][C:38]([NH:40][CH3:41])=[O:39])[C:27]([N:29]([CH2:33][CH2:34][CH3:35])[CH2:30][CH2:31][CH3:32])=[O:28]>C(Cl)Cl>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH:25][CH:26]([CH2:36][CH2:37][C:38]([NH:40][CH3:41])=[O:39])[C:27]([N:29]([CH2:30][CH2:31][CH3:32])[CH2:33][CH2:34][CH3:35])=[O:28])=[O:10]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 10876Furylacrylic acidHCID 10928Ethyl chloroformateHCID 86740989HCID 86740989、化合物

生成物 1

HCID 867409902-[beta-(2-furyl)acrylamido]-N5-methyl-N1,N1-di(n-propyl)pentane-1,5-diamide収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 75 ml of methylene chloride was dissolved 1.5 g of β-(2-furyl)acrylic acid, and 2.7 g of triethylamine and 1.3 g of ethyl chlorocarbonate were successively added thereto dropwise at -25° C. to -20° C. After 30 minutes, 3 g of the DL-2-amino-N5 -methyl-N1,N1 -di(n-propyl)-pentane-1,5-diamide hydrochloride was added to the above solution, and the resulting mixture was subjected to reaction at the same temperature for 30 minutes and at room temperature for 30 minutes. After completion of the reaction, the reaction mixture was washed successively with 30 ml of a 5% aqueous sodium hydroxide solution, 30 ml of diluted hydrochloric acid and 30 ml of water and then dried over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure to obtain 3.1 g (yield 80%) of DL-2-[β-(2-furyl)acrylamido]-N5 -methyl-N1,N1 -di(n-propyl)pentane-1,5-diamide having a melting point of 112°-113° C.

後処理

  1. additionwere successively added
  2. customdropwise at -25° C. to -20° C
  3. customthe resulting mixture was subjected to reaction at the same temperature for 30 minutes and at room temperature for 30 minutes
  4. customAfter completion of the reaction
  5. washthe reaction mixture was washed successively with 30 ml of a 5% aqueous sodium hydroxide solution, 30 ml of diluted hydrochloric acid and 30 ml of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-47a1a8fa8c3e452ea1b4ee37c4296f87
出典データセット
uspto-grants-1986_09
特許番号
US04610983

反応ノート

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