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

HRID 1106195ノート

反応式

HRID 1106195 の反応式
[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]

参加物

4

反応物 3

HCID 962WaterHCID 3283Diethyl EtherHCID 95893-Acetylpyridine

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3ac83655684a4301aef8207c0959ee15
出典データセット
uspto-grants-1982_01
特許番号
US04312368

反応ノート

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