Lithium Hydroxide → 2-(2,3,4-Trifluoroanilino)propionic acid

HRID 8442

반응식

HRID 8442 반응식
[F:1][C:2]1[C:14]([F:15])=[C:13]([F:16])[CH:12]=[CH:11][C:3]=1[NH:4][CH:5]([CH3:10])[C:6]([O:8]C)=[O:7].[OH-].[Li+]>CO>[F:1][C:2]1[C:14]([F:15])=[C:13]([F:16])[CH:12]=[CH:11][C:3]=1[NH:4][CH:5]([CH3:10])[C:6]([OH:8])=[O:7]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 22015876Methyl2-(2,3,4-trifluoroanilino)propionate

생성물 1

HCID 220158662-(2,3,4-Trifluoroanilino)propionic acid수율 99.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl 2-(2,3,4-trifluoroanilino)propionate (46.64 g) was dissolved in methanol (130 ml) and an aqueous solution (3 mol/l; 100 ml) of lithium hydroxide was slowly added thereto at 0° C. After stirring at room temperature for 3 hours, the solvent was evaporated. After adding water, the residue was washed with chloroform. Next, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value reached 1. Then the aqueous layer was extracted with diisopropyl ether (IPE). The organic layer was dried over anhydrous magnesium sulfate and then the solvent was evaporated to give the title compound (43.7 g) as colorless crystals.

후처리

  1. customat 0° C
  2. customthe solvent was evaporated
  3. additionAfter adding water
  4. washthe residue was washed with chloroform
  5. additionNext, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value
  6. extractionThen the aqueous layer was extracted with diisopropyl ether (IPE)
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-8b10cb0936e1470cb7743fcc2219590f
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087778B2

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