1-Hydroxybenzotriazole → 1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride 1-hydroxybenzotriazole

HRID 1785389ノート

反応式

HRID 1785389 の反応式
[ClH:1].[CH3:2][N:3]([CH3:12])[CH2:4][CH2:5][CH2:6][N:7]=[C:8]=[N:9][CH2:10][CH3:11].[OH:13][N:14]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[N:16]=[N:15]1>ClCCl>[OH:13][N:14]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[N:16]=[N:15]1.[ClH:1].[CH3:12][N:3]([CH3:2])[CH2:4][CH2:5][CH2:6][N:7]=[C:8]=[N:9][CH2:10][CH3:11]

参加物

4

反応物 2

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 865980741-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride 1-hydroxybenzotriazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

The acid (1.2 eq.), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.2 eq.) and 1-hydroxybenzotriazole (1.2 eq.) were dissolved in 20 volumes of dichloromethane and the solution stirred for 5 min at room temperature. A solution of the amine E (1 eq.) in 10 volumes dichloromethane was added to the mixture, which was stirred at room temperature overnight. The solution was washed with saturated aqueous NaHCO3, dried over Na2SO4 and filtered. The dichloromethane was removed in vacuo to give the products which were purified with appropriate eluants as shown below.

後処理

  1. stirringwas stirred at room temperature overnight
  2. washThe solution was washed with saturated aqueous NaHCO3
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customThe dichloromethane was removed in vacuo
  6. customto give the products which
  7. customwere purified with appropriate eluants

出典と根拠

ORDレコード
ord-5f48bf5a11d14a35a148d2be9dc00330
出典データセット
uspto-grants-2009_03
特許番号
US07504506B2

反応ノート

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