Hydrochloric Acid → 2-Oxocyclohexanecarboxylic acid

HRID 877480

반응식

HRID 877480 반응식
ClC1C=C(Cl)C(Cl)=CC=1N.Cl.N([O-])=O.[Na+].[O:16]=[C:17]1[CH2:22][CH2:21][CH2:20][CH2:19][CH:18]1[C:23]([O:25]CC)=[O:24].[OH-].[Na+]>O>[O:16]=[C:17]1[CH2:22][CH2:21][CH2:20][CH2:19][CH:18]1[C:23]([OH:25])=[O:24]

참가 물질

7

반응물 5

HCID 313Hydrochloric Acid2회HCID 124872,4,5-TrichloroanilineHCID 14798Sodium HydroxideHCID 95543Ethyl 2-oxocyclohexanecarboxylateHCID 23668193Sodium Nitrite

생성물 1

HCID 99421712-Oxocyclohexanecarboxylic acid

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

To a solution of 2,4,5-trichloroaniline (2.48 g, 12.6 mmol) in H2O (5 mL), cooled to 0° C., conc. HCl (7.5 mL) was added, and then stirred for 20 min. NaNO2 (0.87 g, 12.0 mmol) dissolved in water (5 mL), was added slowly and the reaction was continued at 0° C. for 1 h, filtered and the filtrate was used further. In another setup, ethyl 2-oxocyclohexanecarboxylate (2.0 g, 12.0 mmol) was added to 5N NaOH (0.56 g) and stirred for 16 h. The reaction mixture was cooled to 0° C., conc. HCl (1.2 mL) was added slowly, stirred for another 45 min. to obtain 2-oxocyclohexanecarboxylic acid which was added to the filtrate (prepared above) at 0° C. The resulting yellow solid precipitate was filtered, air dried to give the title compound (1.7 g, 44%) which was used in the next step without any spectroscopic analysis.

후처리

  1. additionwas added slowly
  2. waitthe reaction was continued at 0° C. for 1 h
  3. filtrationfiltered
  4. stirringstirred for 16 h
  5. stirringstirred for another 45 min.

출처 및 근거

ORD 기록
ord-abdaac3e628b4d67a4222c8d68300ce8
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987319B2

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