Ammonium Chloride → HCID 118308685、化合物

HRID 923479ノート

反応式

HRID 923479 の反応式
[CH3:1][N:2]1[CH:6]=[C:5]([C:7](=[O:13])[C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:4]=[N:3]1.[CH3:14][Mg]Br.C(OCC)C.[Cl-].[NH4+]>C1COCC1>[OH:13][C:7]([C:5]1[CH:4]=[N:3][N:2]([CH3:1])[CH:6]=1)([CH3:14])[C:8]([O:10][CH2:11][CH3:12])=[O:9]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 47002973ethyl 2-(1-methyl-1H-pyrazol-4-yl)-2-oxoacetateHCID 178467822HCID 178467822、化合物

生成物 1

HCID 118308685HCID 118308685、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Under an argon atmosphere, to a solution of 500 mg of ethyl (1-methyl-1H-pyrazol-4-yl)(oxo)acetate that had been cooled in a dry ice-acetone bath in 7.5 ml of THF was added 1.56 ml of a 3.0 M methyl magnesium bromide/diethyl ether solution, followed by stirring for 1 hour. To the reaction mixture was added a saturated aqueous ammonium chloride solution, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 302 mg of ethyl 2-hydroxy-2-(1-methyl-1H-pyrazol-4-yl)propanoate.

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was then evaporated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e5f4da5c04e240a18a0be4a11b6e794c
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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