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

HRID 248333

반응식

HRID 248333 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 57417360Sodium chloride; water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-29387480911a4d3f8f2be171f1aacba3
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210080

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