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

HRID 923458ノート

反応式

HRID 923458 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af32dd5262e1497585e08c1ff4b9245b
出典データセット
uspto-grants-2016_03
特許番号
US09278968B2

反応ノート

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