Lithium amide → HCID 21330294, 화합물

HRID 616543

반응식

HRID 616543 반응식
[CH2:1]([C:3]1([CH3:14])[CH:8]([CH3:9])[CH:7]([OH:10])[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4]1)[CH3:2].[C:15]([C:19]1[CH:28]=[CH:27][C:22]([C:23](OC)=[O:24])=[CH:21][CH:20]=1)([CH3:18])([CH3:17])[CH3:16].[NH2-].[Li+]>CCCCCCC>[C:15]([C:19]1[CH:20]=[CH:21][C:22]([C:23]([O:10][CH:7]2[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4][C:3]([CH2:1][CH3:2])([CH3:14])[CH:8]2[CH3:9])=[O:24])=[CH:27][CH:28]=1)([CH3:18])([CH3:16])[CH3:17]

참가 물질

5

반응물 3

HCID 24532Lithium amideHCID 97433Methyl p-tert-butylbenzoateHCID 221822412,6-Diethyl-2,3,6-trimethylpiperidin-4-ol2회

생성물 1

HCID 21330294HCID 21330294, 화합물수율 104.2%

시약·촉매·용매 1

HCID 8900Heptane용매

실험 절차

15.0 g of 2,6-diethyl-2,3,6-trimethyl-4-piperidinol (Compound 1) and 16.0 g of methyl p-t-butylbenzoate were dissolved in 500 ml of heptane. 1.5 g of lithium amide were then added to the solution and the mixture was refluxed by heating in a flask equipped with a Dean-Stark separator. 1.5 g of methanol were first removed and this was followed by 200 ml of heptane, which distilled off over a period of 3 hours. After cooling the reaction mixture, it was washed with water and dried over magnesium sulphate; the solvent was then removed by evaporation under reduced pressure. The residue was distilled under reduced pressure, giving 28.2 g of the title compound as a colourless liquid (bp 176° - 178° C/0.008 mmHg).

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureby heating in a flask
  3. customequipped with a Dean-Stark separator
  4. custom1.5 g of methanol were first removed
  5. distillationdistilled off over a period of 3 hours
  6. temperatureAfter cooling the reaction mixture, it
  7. washwas washed with water
  8. dry with materialdried over magnesium sulphate
  9. customthe solvent was then removed by evaporation under reduced pressure
  10. distillationThe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-d370690fe33242139b3c91d1546af39b
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04075165

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