Methanol → HCID 14794002、化合物

HRID 2247812ノート

反応式

HRID 2247812 の反応式
C([CH:6]1[CH:11]([CH2:12][CH2:13][C:14]([O:17][CH3:18])([CH3:16])[CH3:15])[CH2:10][CH2:9][CH2:8][C:7]1=[O:19])(OCC)=O.[OH-].[K+].CO>O>[CH3:18][O:17][C:14]([CH3:16])([CH3:15])[CH2:13][CH2:12][CH:11]1[CH2:10][CH2:9][CH2:8][C:7](=[O:19])[CH2:6]1

参加物

5

反応物 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 14794005HCID 14794005、化合物

生成物 1

HCID 14794002HCID 14794002、化合物収率 19.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Crude 2-carbethoxy-3-(3-methoxy-3-methylbut-1-yl)cyclohexanone (7.0 g) of example 17 was added to a mixture of potassium hydroxide (3.0 g), methanol (50 mL) and water (50 mL) and heated at reflux 4.5 hours. The cooled mixture was extracted with hexane, the extracts were dried (Na2SO4) and concentrated to an oil which was purified by bulb to bulb distillation, airbath temperature 175~C., 0.1 mm Hg to yield 3-(3-methoxy-3-methylbut-1-yl)cyclohexanone (1.0 g); NMR(CDCl3)δ 1.2(s,6H), 1.2-1.5(m,5H), 1.6-1.8(m,2H), 1.9-2.1(m,3H), 2.2-2.4(m,3H), 3.2(s,3H); IR (neat) 2970, 2950, 1720, 1460, 1370, 1230, 1090 cm-1 ; MS (m/e) 41, 55, 73, 110, 133, 151, 183, 184.

後処理

  1. temperatureheated
  2. temperatureat reflux 4.5 hours
  3. extractionThe cooled mixture was extracted with hexane
  4. dry with materialthe extracts were dried (Na2SO4)
  5. concentrationconcentrated to an oil which
  6. distillationwas purified by bulb to bulb distillation, airbath temperature 175~C

出典と根拠

ORDレコード
ord-527d164731a94fb38506953c5d25858e
出典データセット
uspto-grants-1991_08
特許番号
US05037802

反応ノート

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