Methanol → 4-dipropylaminomethylbenzyl Alcohol

HRID 1173931ノート

反応式

HRID 1173931 の反応式
[CH2:1]([N:4]([CH2:8][C:9]1[CH:18]=[CH:17][C:12]([C:13](OC)=[O:14])=[CH:11][CH:10]=1)[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3].[H-].[Al+3].[Li+].[H-].[H-].[H-].CO.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1COCC1>[CH2:1]([N:4]([CH2:8][C:9]1[CH:18]=[CH:17][C:12]([CH2:13][OH:14])=[CH:11][CH:10]=1)[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3]

参加物

6

反応物 4

HCID 887MethanolHCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 23079192Methyl 4-dipropylaminomethylbenzoate

生成物 1

HCID 669412924-dipropylaminomethylbenzyl Alcohol収率 92%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The compound (1.47 g) obtained in Example 80-1 was dissolved in anhydrous THF (50 ml). Then, the solution was added with lithium aluminum hydride (671 mg) in an ice bath, followed by stirring at room temperature for 1 hour. After completion of the reaction, the solution was added with methanol and then added with an aqueous potassium sodium tartrate solution, followed by stirring. The solution was extracted with chloroform and the extract was then washed with saturated saline solution. The organic layer was dried with anhydrous sodium sulfate and the solvent was then distilled off, thereby obtaining the subject compound (1.20 g) as a colorless liquid.

後処理

  1. customAfter completion of the reaction
  2. stirringby stirring
  3. extractionThe solution was extracted with chloroform
  4. washthe extract was then washed with saturated saline solution
  5. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  6. distillationthe solvent was then distilled off

出典と根拠

ORDレコード
ord-002b64d05b774fdf8f1a1753e5ee77ac
出典データセット
uspto-grants-2010_11
特許番号
US07833991B2

反応ノート

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