Water → Ethyl 2-(2-Butyl)-3-hydroxy-3-methyl-3-(3-pyridyl)propionate

HRID 1106195

반응식

HRID 1106195 반응식
[C:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)(=[O:3])[CH3:2].[OH2:10].[CH3:11][CH2:12][O:13][CH2:14][CH3:15]>>[CH3:2][CH:1]([CH:11]([C:1]([OH:3])([CH3:2])[C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)[C:12]([O:13][CH2:14][CH3:15])=[O:10])[CH2:4][CH3:9]

참가 물질

4

반응물 3

HCID 962WaterHCID 3283Diethyl EtherHCID 95893-Acetylpyridine

생성물 1

HCID 54531343Ethyl 2-(2-Butyl)-3-hydroxy-3-methyl-3-(3-pyridyl)propionate수율 74.5%

실험 절차

To the above solution is added, with stirring, a solution of 3-acetylpyridine (24.2 grams, 0.2 mole) in 80 milliliters of ether. The mixture is stirred for 15 minutes at -78° C. and then allowed to warm up to room temperature (2 hours). Water is added and the ether layer is separated, washed with water, dried with magnesium sulfate and evaporated under reduced pressure to give an oil which weighs 48.0 grams. The oil is distilled in a Kugelrohr apparatus to yield 39.5 grams (74.5%) of the pure product, b.p. 95°-96° C. (air bath temperature) at 0.05 mm Hg.

후처리

  1. additionTo the above solution is added
  2. stirringThe mixture is stirred for 15 minutes at -78° C.
  3. customthe ether layer is separated
  4. washwashed with water
  5. dry with materialdried with magnesium sulfate
  6. customevaporated under reduced pressure
  7. customto give an oil which
  8. distillationThe oil is distilled in a Kugelrohr apparatus

출처 및 근거

ORD 기록
ord-3ac83655684a4301aef8207c0959ee15
출처 데이터셋
uspto-grants-1982_01
특허 번호
US04312368

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