Methanol → HCID 14794002、化合物

HRID 483705ノート

反応式

HRID 483705 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-3ba7a474168a42e68ae6c4622c1abb9d
出典データセット
uspto-grants-1993_07
特許番号
US05225608

反応ノート

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