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

HRID 464618ノート

反応式

HRID 464618 の反応式
[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]

参加物

5

反応物 3

HCID 8014N-MethylethylenediamineHCID 8471TriethylamineHCID 10387Benzyl chloroformate

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d02c5d38b2684ab5809f153648e76a7d
出典データセット
uspto-grants-1985_10
特許番号
US04548815

反応ノート

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