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Water → Benzyl 2-(methylamino)ethylcarbamate

HRID 2066388
ノート
印刷プレビュー

反応式

HRID 2066388 の反応式
[CH3:1][NH:2][CH2:3][CH2:4][NH2:5].[C:6](N1C(=O)CCC1=O)([O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:7].O.C(Cl)(Cl)Cl>O1CCOCC1>[CH3:1][NH:2][CH2:3][CH2:4][NH:5][C:6](=[O:7])[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6212ChloroformHCID 8014N-MethylethylenediamineHCID 3826287Benzyl 2,5-dioxopyrrolidine-1-carboxylate

生成物 1

HCID 10822258Benzyl 2-(methylamino)ethylcarbamate収率 4.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

N-Methylethylenediamine (2.0 g) was dissolved in dioxane (20 ml), the solution was added with N-carbobenzoxysuccinimide (8.07 g), and the mixture was stirred at room temperature for 4 days. The reaction mixture was added with distilled water and chloroform, the layers were separated, and the organic layer was dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1 to 2:1), and then purified again by silica gel column chromatography (chloroform:methanol:28% aqueous ammonia=30:1:0.1) to obtain the title compound (243 mg).

後処理

  1. customthe layers were separated
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1 to 2:1)
  6. custompurified again by silica gel column chromatography (chloroform:methanol:28% aqueous ammonia=30:1:0.1)

出典と根拠

ORDレコード
ord-8f6ebaae1c2e436fb4d6c409df3c04a3
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08293715B2

反応ノート

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