Hydrochloric Acid → HCID 10704523、化合物

HRID 129160ノート

反応式

HRID 129160 の反応式
C(O[CH:4](OCC)[CH2:5][NH:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=1)=[O:8])C.Cl.[OH-].[Na+]>CO.O>[F:19][C:16]([F:17])([F:18])[C:13]1[CH:12]=[CH:11][C:10]([N:9]2[CH:4]=[CH:5][NH:6][C:7]2=[O:8])=[CH:15][CH:14]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 10805622HCID 10805622、化合物

生成物 1

HCID 10704523HCID 10704523、化合物収率 74.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

1-(2,2-Diethoxyethyl)-3-(4-trifluoromethylphenyl)urea (9.2 g, 28.7 mmol) was dissolved in a mixture of 113 ml of methanol and 57 ml of water. To the reaction solution was added 67.5 ml of 0.48N hydrochloric acid and the mixture was stirred for 48 hours at room temperature. To the reaction solution was added 1N sodium hydroxide to adjust pH to 7, followed by being concentrated under reduced pressure. The residue was extracted with ethyl acetate (100 ml×4). The extracts were combined, washed with water and saturated aqueous solution of sodium chloride successively, dried over magnesium sulfate and distilled off. The crystals thus separated out were recystallized from ethyl acetate-isopropylether to give 4.87 g of 1-(4-trifluoromethylphenyl)-2(1H,3H)-imidazolone (74%) as colorless prisms.

後処理

  1. concentrationby being concentrated under reduced pressure
  2. extractionThe residue was extracted with ethyl acetate (100 ml×4)
  3. washwashed with water and saturated aqueous solution of sodium chloride successively
  4. dry with materialdried over magnesium sulfate
  5. distillationdistilled off
  6. customThe crystals thus separated out

出典と根拠

ORDレコード
ord-f2c0de72fdb44448ad4fbbdc2b38179e
出典データセット
uspto-grants-1995_11
特許番号
US05466820

反応ノート

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