Chlorosuccinimide → [4-chloro-2-(1-methylethyl)-1H-imidazol-5-yl]methanol

HRID 439602ノート

反応式

HRID 439602 の反応式
[Cl:1]N1C(=O)CCC1=O.[CH:9]([C:12]1[NH:13][C:14]([CH2:19][OH:20])=[C:15](CO)[N:16]=1)([CH3:11])[CH3:10]>C(O)C>[CH:9]([C:12]1[NH:13][C:14]([CH2:19][OH:20])=[C:15]([Cl:1])[N:16]=1)([CH3:11])[CH3:10]

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 136089212-Isopropyl-4,5-bis(hydroxymethyl) imidazole

生成物 1

HCID 15338147[4-chloro-2-(1-methylethyl)-1H-imidazol-5-yl]methanol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2.81 Grams (21 mmol) of the N-chlorosuccinimide was added little by little to a solution consisting of 3.47 g (20.4 mmol) of a 2-isopropyl-4,5-bis(hydroxymethyl) imidazole and 220 ml of ethanol at a temperature of 40° to 45° C. with stirring over a period of about 25 minutes. The mixture was stirred at the same temperature for two hours to effect the reaction, and then ethanol was distilled off under reduced pressure. The resulting reaction product was washed with water to obtain a pale yellowish powdery crystalline 2-isopropyl-4-chloro-5-(hydroxymethyl) imidazole in an amount of 1.69 g (yield, 47.4%). By using acetonitrile, the recrystallization was effected twice to obtain a colorless crystalline product in pure form. The TLC and spectra of this compound were the same as the properties exhibited by the above-mentioned 2-isopropyl-4-chloro-5-(hydroxymethyl) imidazole.

後処理

  1. stirringThe mixture was stirred at the same temperature for two hours
  2. customthe reaction
  3. distillationethanol was distilled off under reduced pressure
  4. customThe resulting reaction product
  5. washwas washed with water

出典と根拠

ORDレコード
ord-46a536f99f7542169b148789ff81435f
出典データセット
uspto-grants-1996_05
特許番号
US05514811

反応ノート

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