Diethylenetriamine → N,N''-Di-Z-diethylenetriamine

HRID 399367

反応式

HRID 399367 の反応式
[NH2:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH2:7].C(N([CH2:13][CH3:14])CC)C.C([C:17]([O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:18])#N>ClCCl>[CH2:20]([O:19][C:17]([NH:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][C:17]([O:19][CH2:20][C:14]1[CH:13]=[CH:23][CH:22]=[CH:21][CH:26]=1)=[O:18])=[O:18])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 8111DiethylenetriamineHCID 8471TriethylamineHCID 79660Benzyl cyanoformate

生成物 1

HCID 4367374N,N''-Di-Z-diethylenetriamine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

51.5 g (500 mmol) of diethylenetriamine and 139 ml (1 mol) of triethylamine are dissolved in dichloromethane and mixed at -20° C. with 161 g of benzyl cyanoformate (Fluka) in dichloromethane and then stirred overnight at room temperature. After the reaction is completed, concentration by evaporation is performed during draw-off, the residue is taken up in diethyl ether, the organic phase is washed with sodium carbonate solution and dried with sodium sulfate. The filtrate is mixed with hexane, the precipitate is filtered out and dried.

後処理

  1. concentrationconcentration
  2. customby evaporation
  3. washthe organic phase is washed with sodium carbonate solution
  4. dry with materialdried with sodium sulfate
  5. additionThe filtrate is mixed with hexane
  6. filtrationthe precipitate is filtered out
  7. customdried

出典と根拠

ORDレコード
ord-b8b16aaaca1e4eaeb10499e1d4ff9603
出典データセット
uspto-grants-1998_10
特許番号
US05820849

関連ノート

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