Thionyl Chloride → 1-Phenacyl-2-(2-chloroethylamino)benzimidazole hydrochloride

HRID 54691ノート

反応式

HRID 54691 の反応式
S(Cl)([Cl:3])=O.O[CH2:6][CH2:7][NH:8][C:9]1[N:13]([CH2:14][C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:16])[C:12]2[CH:23]=[CH:24][CH:25]=[CH:26][C:11]=2[N:10]=1>C(Cl)(Cl)Cl>[ClH:3].[CH2:14]([N:13]1[C:12]2[CH:23]=[CH:24][CH:25]=[CH:26][C:11]=2[N:10]=[C:9]1[NH:8][CH2:7][CH2:6][Cl:3])[C:15]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:16]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 28501002-{2-[(2-hydroxyethyl)amino]-1H-benzimidazol-1-yl}-1-phenylethanone

生成物 1

HCID 190408301-Phenacyl-2-(2-chloroethylamino)benzimidazole hydrochloride収率 90%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Add 0.7 ml (10 mmol) of freshly distilled thionyl chloride, with stirring, to a suspension of 1.5 g (5 mmol) of the base obtained above in 25 ml of anhydrous chloroform. Heat the resulting solution at reflux for 1 hour. After cooling, the 1-phenacyl-2-(2-chloroethylamino)benzimidazole hydrochloride precipitate is isolated by filtration, washed with petroleum ether and recrystallised from a mixture of ethanol/ether.

後処理

  1. temperatureHeat the resulting solution
  2. temperatureat reflux for 1 hour
  3. temperatureAfter cooling

出典と根拠

ORDレコード
ord-7555846cb41b4fb190495861083de511
出典データセット
uspto-grants-1997_04
特許番号
US05623073

反応ノート

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