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

HRID 363271

반응식

HRID 363271 반응식
[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

참가 물질

5

반응물 3

HCID 8111DiethylenetriamineHCID 8471TriethylamineHCID 79660Benzyl cyanoformate

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-44d657dd93a14d4a9555e1b08402b1a6
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05874061

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