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Ethanol → N,N-Dimethyl-1-(morpholin-2-yl)methanamine--hydrogen chloride (1/2)

HRID 477812
ノート
印刷プレビュー

反応式

HRID 477812 の反応式
[ClH:1].Cl.[CH3:3][N:4]([CH2:6][CH:7]1[O:12][CH2:11][CH2:10][N:9](CC2C=CC=CC=2)[CH2:8]1)[CH3:5].C(O)C>[C].[Pd].O>[ClH:1].[ClH:1].[CH3:3][N:4]([CH2:6][CH:7]1[O:12][CH2:11][CH2:10][NH:9][CH2:8]1)[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 702EthanolHCID 198349682-(N,N-dimethylaminomethyl)-4-benzylmorpholine dihydrochloride

生成物 1

HCID 14652585N,N-Dimethyl-1-(morpholin-2-yl)methanamine--hydrogen chloride (1/2)

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 962Water溶媒

実験手順

A mixture of 22.5 g of 4-benzyl-2-chloromethylmorpholine, 200 ml of ethanol and 200 ml of an aqueouos 26,7% dimethylamine solution is heated at 150° C. for 5 hours in an autoclave. After completion of the reaction, the solvent is distilled off under reduced pressure. After adding water, the residue is extracted with toluene three times. The extract is washed with water and dried over anhydrous magnesium sulfate. The solvent is distilled off under reduced pressure and the residue is treated with 37% hydrochloric acid-ethanol to give 2-(N,N-dimethylaminomethyl)-4-benzylmorpholine dihydrochloride as white crystals. A mixture of 22.9 g of the hydrochloride compound, 200 ml of ethanol and 100 ml of water is subjected to catalytic reduction with 2.3 g of 10% palladium-carbon at ordinary temperature and atmospheric pressure. After absorbing a theoretical volume of the hydrogen, the catalyst is filtered off and the filtrate is concentrated under reduced pressure. The obtained residue is treated with ethanol to give 2-(N,N-dimethylaminomethyl)morpholine dihydrochloride as white crystals, melting at 270°-271° C.

後処理

  1. customAfter absorbing a theoretical volume of the hydrogen
  2. filtrationthe catalyst is filtered off
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. additionThe obtained residue is treated with ethanol

出典と根拠

ORDレコード
ord-828af3ec830544b799d6ad37a30f4afe
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04889857

反応ノート

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