Bis(2-chloroethyl)amine hydrochloride → Eltoprazine

HRID 365292ノート

反応式

HRID 365292 の反応式
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([NH2:11])[C:5]=2[O:4][CH2:3][CH2:2]1.Cl.Cl[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]Cl>ClC1C=CC=CC=1>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[C:5]=2[O:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 522769Bis(2-chloroethyl)amine hydrochlorideHCID 117883872,3-Dihydro-1,4-benzodioxin-5-amine

生成物 1

HCID 65853Eltoprazine収率 90.8%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

The solution of the product of example 13 (1.50 g, 0.010 mol) and bis(2-chloroethyl)amine hydrochloride (1.77 g 0.01 mol) in chlorobenzene (20 ml) was heated under reflux for 24 h, cooled to room temperature and evaporated in vacuo. The white solid was dissolved in aqueous sodium hydroxide (100 ml) and extracted into ethyl acetate (3×50 ml). The extracts were dried (MgSO4) and evaporated in vacuo to give the product (2.00 g).

後処理

  1. temperatureunder reflux for 24 h
  2. customevaporated in vacuo
  3. dissolutionThe white solid was dissolved in aqueous sodium hydroxide (100 ml)
  4. extractionextracted into ethyl acetate (3×50 ml)
  5. dry with materialThe extracts were dried (MgSO4)
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-c5756552bbd3491fba645fbf4c5e7481
出典データセット
uspto-grants-2000_10
特許番号
US06127357

反応ノート

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