Methanol → HCID 14794002, 화합물

HRID 329485노트

반응식

HRID 329485 반응식
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

참가 물질

5

반응물 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 14794005HCID 14794005, 화합물

생성물 1

HCID 14794002HCID 14794002, 화합물수율 19.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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)δ1.2(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.

후처리

  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., 0.1 mm Hg

출처 및 근거

ORD 기록
ord-0c57de15ff2d490e9836bee545ba8e89
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04891447

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