Sodium sulfate decahydrate → HCID 178483465、化合物

HRID 2225519

反応式

HRID 2225519 の反応式
[CH3:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([N-:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]([CH3:15])[CH3:14])[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>[CH3:15][N:13]([CH3:14])[CH2:12][CH2:11][CH2:10][CH2:9][NH:8][C@H:5]1[CH2:6][CH2:7][C@H:2]([CH3:1])[CH2:3][CH2:4]1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 178483464HCID 178483464、化合物

生成物 1

HCID 178483465HCID 178483465、化合物収率 43.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

13.1 g of N-(trans-4-methylcyclohexyl ) -4-dimethylaminobutylamide (Example 73) was dissolved in 100 ml of THF. Under an argon stream, the solution was added dropwise to a solution of 7.5 g of lithium aluminum hydride suspended in 400 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, 22 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, yielding an oily substance. This substance was subjected to vacuum distillation, yielding 5.7 g of N-(4-dimethylaminobutyl)-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. customyielding an oily substance
  10. distillationThis substance was subjected to vacuum distillation

出典と根拠

ORDレコード
ord-4922bd34b49f4b1fbd9a29e82b835f1e
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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