N-Methylethylenediamine → N-Methyl-N,N'-dibenzyloxycarbonyl-1,2-diaminoethane

HRID 464618노트

반응식

HRID 464618 반응식
[CH3:1][NH:2][CH2:3][CH2:4][NH2:5].C(N([CH2:11][CH3:12])CC)C.Cl[C:14]([O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:15]>C(Cl)(Cl)Cl>[CH3:1][N:2]([C:14]([O:16][CH2:17][C:12]1[CH:11]=[CH:20][CH:19]=[CH:18][CH:23]=1)=[O:15])[CH2:3][CH2:4][NH:5][C:14]([O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:15]

참가 물질

5

반응물 3

HCID 8014N-MethylethylenediamineHCID 8471TriethylamineHCID 10387Benzyl chloroformate

생성물 1

HCID 20236398N-Methyl-N,N'-dibenzyloxycarbonyl-1,2-diaminoethane수율 86.6%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a stirred solution of N-Methyl-1,2-diaminoethane (7.4 gm) and triethylamine (20.2 gm) in chloroform (50 ml) at 0° was added dropwise over 30 minutes benzyl chloroformate (34.1 gm). The mixture was then left to warm to room temperature over one hour. The organic solution was then washed with water, citric acid solution, sodium bicarbonate solution and finally water again. The chloroform solution was dried over magnesium sulphate and evaporated to give a yellow oil (29.6 g).

후처리

  1. waitThe mixture was then left
  2. washThe organic solution was then washed with water, citric acid solution, sodium bicarbonate solution and finally water again
  3. dry with materialThe chloroform solution was dried over magnesium sulphate
  4. customevaporated

출처 및 근거

ORD 기록
ord-d02c5d38b2684ab5809f153648e76a7d
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04548815

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