Sodium sulfate decahydrate → HCID 178483797、化合物

HRID 2225522

反応式

HRID 2225522 の反応式
[CH3:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:9](=O)[CH2:10][N:11]([CH3:13])[CH3:12])[CH2:4][CH2:3]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH3:12][N:11]([CH3:13])[CH2:10][CH2:9][NH:8][C@H:5]1[CH2:4][CH2:3][C@H:2]([CH3:1])[CH2:7][CH2:6]1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 178483959HCID 178483959、化合物

生成物 1

HCID 178483797HCID 178483797、化合物収率 48.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

8.5 g of N-(trans-4-methylcyclohexyl)-2-dimethylaminoacetamide was dissolved in 100 ml of THF. Under an argon stream, the solution was added dropwise to a solution of 3.6 g of lithium aluminum hydride suspended in 200 ml of THF under ice-cooling. After the addition, the solution was reacted for 8 hours, while it was refluxed. After reaction, the solution was allowed to cool to room temperature. Then, 10 g of sodium sulfate decahydrate was added to the solution under ice-cooling. The solution was stirred for 1 hour, and the precipitate was filtered out. The solvent was removed in vacuo to obtaine an oily substance. This substance was refined by vacuum distillation, yielding 3.8 g of N-(2-dimethylaminoethyl)-trans-4-methylcyclohexylamine as a colorless oil, which had the following physiochemical properties:

後処理

  1. temperaturecooling
  2. additionAfter the addition
  3. customthe solution was reacted for 8 hours, while it
  4. temperaturewas refluxed
  5. customAfter reaction
  6. temperaturecooling
  7. filtrationthe precipitate was filtered out
  8. customThe solvent was removed in vacuo
  9. distillationThis substance was refined by vacuum distillation

出典と根拠

ORDレコード
ord-a98b033b1a784888b2a2f4a3155cd5d6
出典データセット
uspto-grants-1994_09
特許番号
US05344845

関連ノート

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