Diethyl Ether → N,N-Bis(2-chloroethyl)benzylamine hydrochloride

HRID 343496

反応式

HRID 343496 の反応式
S(Cl)([Cl:3])=O.O[CH2:6][CH2:7][N:8]([CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:9]CO.C(OCC)C.[CH:24]([Cl:27])(Cl)Cl>>[ClH:3].[Cl:3][CH2:6][CH2:7][N:8]([CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:9][CH2:24][Cl:27]

参加物

5

反応物 4

HCID 3283Diethyl EtherHCID 6212Chloroform2 回HCID 75532,2'-((Phenylmethyl)imino)bisethanolHCID 24386Thionyl Chloride

生成物 1

HCID 2777881N,N-Bis(2-chloroethyl)benzylamine hydrochloride

実験手順

Combine thionyl chloride (25.4 g, 130 mmol) and chloroform (20 mL). Add over about 1 hour, a solution of N,N-bis(2-hydroxyethyl)benzylamine (25.4 g, 130 mmol) in chloroform (20 mL). After the addition is complete, heat to reflux. After 1 hour, cool the reaction mixture to ambient temperature and add diethyl ether to form a solid. Collect the solid by filtration, rinse with diethyl ether, and dry to give N,N-bis(2-chloroethyl)benzylamine hydrochloric acid salt.

後処理

  1. additionAdd over about 1 hour
  2. additionAfter the addition
  3. temperatureheat to reflux
  4. customto form a solid
  5. customCollect the solid
  6. filtrationby filtration
  7. washrinse with diethyl ether
  8. customdry

出典と根拠

ORDレコード
ord-81dc470047bc4c2ca0422c8d8bc03f42
出典データセット
uspto-grants-1999_01
特許番号
US05861417

関連ノート

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