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1H-Imidazole, 5-((3,5-dichlorophenyl)thio)-1-ethyl-4-(1-methylethyl)-2-(2-(phenylmethoxy)ethyl)- → 1H-Imidazole-2-ethanol, 5-((3,5-dichlorophenyl)thio)-1-ethyl-4-(1-methylethyl)-

HRID 1857756
ノート
印刷プレビュー

反応式

HRID 1857756 の反応式
C([O:8][CH2:9][CH2:10][C:11]1[N:12]([CH2:28][CH3:29])[C:13]([S:19][C:20]2[CH:25]=[C:24]([Cl:26])[CH:23]=[C:22]([Cl:27])[CH:21]=2)=[C:14]([CH:16]([CH3:18])[CH3:17])[N:15]=1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>Cl>[Cl:26][C:24]1[CH:25]=[C:20]([S:19][C:13]2[N:12]([CH2:28][CH3:29])[C:11]([CH2:10][CH2:9][OH:8])=[N:15][C:14]=2[CH:16]([CH3:17])[CH3:18])[CH:21]=[C:22]([Cl:27])[CH:23]=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

4

反応物 2

HCID 4740951H-Imidazole, 5-((3,5-dichlorophenyl)thio)-1-ethyl-4-(1-methylethyl)-2-(2-(phenylmethoxy)ethyl)-HCID 516892Sodium Bicarbonate

生成物 1

HCID 4740961H-Imidazole-2-ethanol, 5-((3,5-dichlorophenyl)thio)-1-ethyl-4-(1-methylethyl)-収率 85%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
100 °C

実験手順

In 16 ml of cocentrated hydrochloric acid was dissolved 3.8 g (8.5 mmol) of the benzyl compound (122a), and the mixture was heated at 100° C. for 2 hours. After cooling, the mixture was neutralized with sodium hydrogen carbonate, extracted with ethyl acetate, the extract was washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (1% methanol:ethyl acetate), washed with n-hexane, and filtered to give 2.57 g of 2-[5-(3,5-dichlorophenylthio)-1-ethyl-4-isopropyl-1H-imidazol-2-yl]ethanol (123a) as crystals (yield 85%). mp 80-81° C.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washthe extract was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (1% methanol:ethyl acetate)
  8. washwashed with n-hexane
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-9cdd68e11446406b8abf7246844413a2
出典データセット
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06147097

反応ノート

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