Hydrochloric Acid → HCID 10704523, 화합물

HRID 1491784노트

반응식

HRID 1491784 반응식
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

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 10805622HCID 10805622, 화합물

생성물 1

HCID 10704523HCID 10704523, 화합물수율 74.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-00dfc8e50f224a66bb084cb6f9e991e2
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371101

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