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Diethyl Ether → N'-(2-Amino-2-methylpropyl)-N,N-dimethylsulfuric diamide

HRID 2107570
ノート
印刷プレビュー

反応式

HRID 2107570 の反応式
[NH2:1][CH2:2][C:3]([NH2:6])([CH3:5])[CH3:4].CCOCC.[CH3:12][N:13]([CH3:18])[S:14](Cl)(=[O:16])=[O:15]>C(N(CC)CC)C>[CH3:4][C:3]([NH2:6])([CH3:5])[CH2:2][NH:1][S:14]([N:13]([CH3:18])[CH3:12])(=[O:16])=[O:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 131282-MethylpropylenediamineHCID 83372Dimethylsulphamoyl chloride

生成物 1

HCID 13603865N'-(2-Amino-2-methylpropyl)-N,N-dimethylsulfuric diamide収率 60.4%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

A mixture of 30.7 g (0.35 mol) of 1,2-diamino-2-methylpropane, 150 ml of ether and 50 ml of triethylamine was cooled to 0° C. and 20 g (0.14 mol) of dimethylsulfamoyl chloride was added slowly. The reaction mixture was stirred for 30 minutes and evaporated to dryness. The residue was mixed with water, basified with K2CO3 and evaporated to dryness. Acetone was added and the mixture was filtered. Evaporation of the filtrate gave a solid which was recrystalized from toluene to give 16.5 g (60.3%) of product, mp 77°-78° C. The NMR and IR were consistent with the assigned structure.

後処理

  1. customevaporated to dryness
  2. additionThe residue was mixed with water
  3. customevaporated to dryness
  4. additionAcetone was added
  5. filtrationthe mixture was filtered
  6. customEvaporation of the filtrate
  7. customgave a solid which
  8. customwas recrystalized from toluene

出典と根拠

ORDレコード
ord-de74ef9d955d4bdda0d924e05b050262
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04935421

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート