Hydrochloric Acid → HCID 178526855、化合物

HRID 1092883ノート

反応式

HRID 1092883 の反応式
F[B-](F)(F)F.[O:6]=[N+:7]=[O:8].[Cl:9][C:10]1[NH:11][CH:12]=[CH:13][N:14]=1.C(=O)([O-])O.[Na+].Cl>[N+](C)([O-])=O>[Cl:9][C:10]1[NH:11][CH:12]=[C:13]([N+:7]([O-:8])=[O:6])[N:14]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 27733282-chloro-1H-imidazoleHCID 11073463Nitronium tetrafluoroborate

生成物 1

HCID 178526855HCID 178526855、化合物収率 34.9%

試薬・触媒・溶媒 1

HCID 6375Nitromethane溶媒

実験手順

Nitronium tetrafluoroborate (398 mg) was dissolved in nitromethane (5 ml), next 2-chloroimidazole (205 mg) was added, the reaction mixture was stirred at a room temperature for 1 hour. The reaction mixture was neutralized with an aqueous solution of sodium hydrogencarbonate, then was turned back to acidic by adding hydrochloric acid, the separated 2-chloro-4-nitroimidazole (137 mg) was collected by filtration. The filtrate was extracted with ethyl acetate-methanol, the solid matter obtained from the organic layer was triturated with diethyl ether, 2-chloro-4-nitroimidazole (103 mg) was obtained. The sum of 240 mg (yield: 81.3%) of 2-chloro-4-nitroimidazole was obtained as colorless solid product.

後処理

  1. filtrationthe separated 2-chloro-4-nitroimidazole (137 mg) was collected by filtration
  2. extractionThe filtrate was extracted with ethyl acetate-methanol
  3. customthe solid matter obtained from the organic layer
  4. customwas triturated with diethyl ether

出典と根拠

ORDレコード
ord-ce1bc40b01ae461da076c59eefa182fd
出典データセット
uspto-grants-2012_03
特許番号
US08129544B2

反応ノート

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