Pyridine → 1-(2-Acetoxyethyl)-5-acetylaminopyrazole

HRID 1376411

反応式

HRID 1376411 の反応式
[OH:1][CH2:2][CH2:3][N:4]1[C:8]([NH2:9])=[CH:7][CH:6]=[N:5]1.[C:10](OC(=O)C)(=[O:12])[CH3:11].N1[CH:22]=[CH:21]C=CC=1.C(=O)(O)[O-:24].[Na+]>[Cl-].[Na+].O.C(OCC)(=O)C>[C:10]([O:1][CH2:2][CH2:3][N:4]1[C:8]([NH:9][C:21](=[O:24])[CH3:22])=[CH:7][CH:6]=[N:5]1)(=[O:12])[CH3:11]

参加物

7

反応物 4

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 3202812-(5-amino-1H-pyrazol-1-yl)ethan-1-olHCID 516892Sodium Bicarbonate

生成物 1

HCID 229167651-(2-Acetoxyethyl)-5-acetylaminopyrazole

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

1-(2-Hydroxyethyl)-5-aminopyrazole (5 g) was added to acetic anhydride (14.7 ml) under stirring and ice-cooling, and pyridine (6.3 ml) was added thereto. The mixture was stirred for 2 hours at 25° C. The reaction mixture was added to a mixture of ethyl acetate (50 ml) and brine (50 ml). Then, the mixture was adjusted to pH 7.0 with an aqueous solution of sodium bicarbonate. The aqueous layer was extracted with a mixture of ethyl acetate and tetrahydrofuran. The extract was dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure to give 1-(2-acetoxyethyl)-5-acetylaminopyrazole (5.98 g).

後処理

  1. temperatureice-cooling
  2. stirringThe mixture was stirred for 2 hours at 25° C
  3. extractionThe aqueous layer was extracted with a mixture of ethyl acetate and tetrahydrofuran
  4. dry with materialThe extract was dried over magnesium sulfate
  5. filtrationThe magnesium sulfate was filtered off
  6. customthe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-03b639c79c4f4bd4a2742ffe81493c62
出典データセット
uspto-grants-1997_09
特許番号
US05663163

関連ノート

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