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(4-Benzylmorpholin-2-yl)methanamine → (S)-(4-benzylmorpholin-2-yl)methanamine

HRID 324957
ノート
印刷プレビュー

反応式

HRID 324957 の反応式
[NH2:1][CH2:2][CH:3]1[O:8][CH2:7][CH2:6][N:5]([CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:4]1>C(O)C>[NH2:1][CH2:2][C@@H:3]1[O:8][CH2:7][CH2:6][N:5]([CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 2776360(4-Benzylmorpholin-2-yl)methanamine

生成物 1

HCID 6932054(S)-(4-benzylmorpholin-2-yl)methanamine収率 42.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(RS)-2-Aminomethyl-4-benzylmorpholine (326.1 g) was dissolved in ethanol (3 L) and dibenzoyl-D-tartaric monohydrate (535 g) was added. The mixture was refluxed for dissolution and then left standing at room temperature for 16 hours. The precipitated crystals were collected by filtration and recrystallized from a mixed solvent of ethanol:water=25:1. The obtained crystals were suspended in water (1.2 L) and aqueous sodium hydroxide solution was added with stirring to make the suspension basic, which was followed by extraction with chloroform. The chloroform layer was dried over anhydrous magnesium sulfate and the solvent was distilled off to give 138.4 g of (S)-2-aminomethyl-4-benzylmorpholine as a colorless oil.

後処理

  1. temperatureThe mixture was refluxed for dissolution
  2. waitleft
  3. filtrationThe precipitated crystals were collected by filtration
  4. customrecrystallized from a mixed solvent of ethanol
  5. additionaqueous sodium hydroxide solution was added
  6. extractionwas followed by extraction with chloroform
  7. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-0e20dc9cdaf94006819cf687afc16f90
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06221864B1

反応ノート

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