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

HRID 903607ノート

反応式

HRID 903607 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-e57a32ec316f4e52b03a1134704acf5a
出典データセット
uspto-grants-1980_10
特許番号
US04228174

反応ノート

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