Hydrochloric Acid → Ethyl 2-amino-2-(1-methyl-1H-pyrazol-4-yl)acetate

HRID 923458노트

반응식

HRID 923458 반응식
C1(C(=[N:14][CH:15]([C:21]2[CH:22]=[N:23][N:24]([CH3:26])[CH:25]=2)[C:16]([O:18][CH2:19][CH3:20])=[O:17])C2C=CC=CC=2)C=CC=CC=1.Cl>O1CCOCC1>[NH2:14][CH:15]([C:21]1[CH:22]=[N:23][N:24]([CH3:26])[CH:25]=1)[C:16]([O:18][CH2:19][CH3:20])=[O:17]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 118318070ethyl [(diphenylmethylene)amino](1-methyl-1H-pyrazol-4-yl)acetate

생성물 1

HCID 60797101Ethyl 2-amino-2-(1-methyl-1H-pyrazol-4-yl)acetate수율 75.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 228 mg of ethyl [(diphenylmethylene)amino](1-methyl-1H-pyrazol-4-yl)acetate in 2.8 ml of 1,4-dioxane was added 1.9 ml of 1 M hydrochloric acid, followed by stirring at room temperature for 2.5 hours. The reaction mixture was concentrated under reduced pressure, the obtained residue was washed with diethyl ether, and to the aqueous layer was added a saturated aqueous sodium hydrogen carbonate solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and the solvent was then evaporated under reduced pressure to obtain 91 mg of ethyl amino(1-methyl-1H-pyrazol-4-yl)acetate.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. washthe obtained residue was washed with diethyl ether
  3. additionto the aqueous layer was added a saturated aqueous sodium hydrogen carbonate solution
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. customthe solvent was then evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-af32dd5262e1497585e08c1ff4b9245b
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278968B2

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