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Water → 2-hydroxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole

HRID 8405
ノート
印刷プレビュー

反応式

HRID 8405 の反応式
C([O:8][CH2:9][C:10]1[N:11]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)[CH:12]=[C:13]([CH:15]([CH3:17])[CH3:16])[N:14]=1)C1C=CC=CC=1.O.C1(C)C=CC=CC=1>Cl>[OH:8][CH2:9][C:10]1[N:11]([C:18]2[CH:19]=[CH:20][N:21]=[CH:22][CH:23]=2)[CH:12]=[C:13]([CH:15]([CH3:17])[CH3:16])[N:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 1140TolueneHCID 220157572-Benzyloxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole

生成物 1

HCID 220157552-hydroxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole収率 86.6%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
85 °C

実験手順

The compound (5) (20.0 g, 62.2 mmol) was suspended in 35% aqueous hydrochloric acid (100 ml). The solution was heated at 85° C. and stirred for 1 hour. The reaction mixture was cooled down to room temperature and water (100 ml) and toluene (44 ml) were added thereto with stirring. The aqueous layer was separated and neutralized with 30% aqueous sodium hydroxide, to which ethyl acetate (30 ml) was added with stirring. The obtained slurry was filtered, washed with cold water and dried to yield 2-hydroxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole (9) (11.7 g). Yield 81.4%.

後処理

  1. temperatureThe reaction mixture was cooled down to room temperature
  2. stirringwith stirring
  3. customThe aqueous layer was separated
  4. additionwas added
  5. stirringwith stirring
  6. filtrationThe obtained slurry was filtered
  7. washwashed with cold water
  8. customdried

出典と根拠

ORDレコード
ord-817f567d751f49859e698e37d51e69b5
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07087764B2

反応ノート

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