Lithium amide → HCID 21330294、化合物

HRID 616543

反応式

HRID 616543 の反応式
[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]

参加物

5

反応物 3

HCID 24532Lithium amideHCID 97433Methyl p-tert-butylbenzoateHCID 221822412,6-Diethyl-2,3,6-trimethylpiperidin-4-ol2 回

生成物 1

HCID 21330294HCID 21330294、化合物収率 104.2%

試薬・触媒・溶媒 1

HCID 8900Heptane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d370690fe33242139b3c91d1546af39b
出典データセット
uspto-grants-1978_02
特許番号
US04075165

関連ノート

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