Sodium Hydroxide → Ethyl 2-(4-amino-3-fluorophenyl)acetate

HRID 889486노트

반응식

HRID 889486 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8](C(OCC)=O)[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:4][C:3]=1[F:19].[OH-].[Na+]>C(O)C.O>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:4][C:3]=1[F:19]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 58399565Diethyl (4-amino-3-fluorophenyl)propanedioate

생성물 1

HCID 59760056Ethyl 2-(4-amino-3-fluorophenyl)acetate

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

Diethyl (4-amino-3-fluorophenyl)propanedioate (11.85 g, 44.1 mmol) was dissolved in ethanol (80 ml) and treated with NaOH (2.6 g, 1.5 eq) dissolved in 18 ml of water to give a pink solution. This was heated to 90° C. for 1 hour until complete. Heating continued for 1 further hour, and then cooled to room temperature. Solvent evaporated and acidified with 2N HCl. Extracted with ethyl acetate (3×100 ml). Organics washed with brine and dried over MgSO4. Evaporated to give the title compound as a yellow oil which crystallised slowly on standing (6.6 g).

후처리

  1. customto give a pink solution
  2. temperatureHeating
  3. temperaturecooled to room temperature
  4. customSolvent evaporated
  5. extractionExtracted with ethyl acetate (3×100 ml)
  6. washOrganics washed with brine
  7. dry with materialdried over MgSO4
  8. customEvaporated

출처 및 근거

ORD 기록
ord-4ce4dac263bb431db9d0bf41181923ea
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252833B2

반응 노트

불러오는 중…