Ethanol, 2,2'-(1,2-ethanediyldiimino)bis- → 1,2-Ethanediamine, N,N'-bis(2-chloroethyl)-, dihydrochloride

HRID 742387ノート

反応式

HRID 742387 の反応式
[Cl:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][Cl:10].OCCNCCNCCO>O=S(Cl)Cl>[ClH:1].[ClH:1].[Cl:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][Cl:10]

参加物

4

反応物 2

HCID 78179Ethanol, 2,2'-(1,2-ethanediyldiimino)bis-HCID 409899N,N'-Bis(2-chloroethyl)ethylenediamine

生成物 1

HCID 30474461,2-Ethanediamine, N,N'-bis(2-chloroethyl)-, dihydrochloride

試薬・触媒・溶媒 1

HCID 24386Thionyl Chloride溶媒

実験手順

N,N'-Bis(2-chloroethyl)ethylenediamine (BCE) A solution of N,N'-bis(2-hydroxyethyl)ethylenediamine (5.4 g, 0.036 mol) in SOCl2 (60 mL) was heated at 90° C. for 2 h, then stirred at room temperature for 24 h. Excess SOCl2 was then removed under reduced pressure, and the residue was triturated with isopropanol. Crystallisation from boiling isopropanol (800 mL) containing just enough water to dissolve the solids gave N,N'-bis(2-chloroethyl)ethylenediamine dihydrochloride (BCE.2HCl).

後処理

  1. customExcess SOCl2 was then removed under reduced pressure
  2. customthe residue was triturated with isopropanol
  3. customCrystallisation
  4. additioncontaining just enough water
  5. dissolutionto dissolve the solids

出典と根拠

ORDレコード
ord-69d12510b9c14d179279c2e24e7d2eb4
出典データセット
uspto-grants-1996_09
特許番号
US05554648

反応ノート

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