Potassium Hydroxide → HCID 19904422, 화합물

HRID 2372419노트

반응식

HRID 2372419 반응식
[C:1]([C:6]1([C:13](OCC)=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1=[O:12])(OCC)=[O:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[K+].P([O-])([O-])(O)=O.[K+].[K+].P([O-])(O)(O)=O.[K+]>CCOCC.O>[OH:14][CH2:13][C:6]1([CH2:1][OH:2])[CH2:11][CH2:10][CH2:9][CH2:8][CH:7]1[OH:12]

참가 물질

8

반응물 5

HCID 14797Potassium HydroxideHCID 24450Potassium Phosphate, DibasicHCID 224023Diethyl 2-oxocyclohexane-1,1-dicarboxylateHCID 516951Monobasic potassium phosphateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 19904422HCID 19904422, 화합물수율 60.5%

시약·촉매·용매 2

HCID 962Water용매2회HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 2,2-dicarbethoxycyclohexanone (3.0 g.) in dry ether (15 ml.) was added dropwise to a stirred suspension of lithium aluminium hydride (1.4 g.) in dry ether (50 ml.) at 0°, under nitrogen. The mixture was refluxed, with stirring, for six hours. Potassium hydroxide (6 g.) in water (100 ml) was added to the stirred mixture. Dipotassium hydrogen phosphate (4.2 g.) and potassium dihydrogen phosphate (3.3 g.) in water (50 ml.) was added. Ether was removed by passing a current of nitrogen through the mixture. The resultant slurry was acidified with glacial acetic acid and the solid was filtered off. The filtrate was evaporated in vacuo. The residue was extracted with acetone and the solution was evaporated in vacuo. 2,2Di-(hydroxymethyl)-cyclohexanol (1.2 g.) was obtained as a pale yellow oil.

후처리

  1. temperatureThe mixture was refluxed
  2. customEther was removed
  3. filtrationthe solid was filtered off
  4. customThe filtrate was evaporated in vacuo
  5. extractionThe residue was extracted with acetone
  6. customthe solution was evaporated in vacuo

출처 및 근거

ORD 기록
ord-b58d505661ee43bc907e035160e47acb
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05098929

반응 노트

불러오는 중…