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Ethylamine → 1-(3,4-Methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride

HRID 26002
ノート
印刷プレビュー

反応式

HRID 26002 の反応式
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH:10]([OH:13])[CH2:11][Cl:12])=[CH:4][C:3]=2[O:2]1.[CH2:14]([NH2:16])[CH3:15]>C(O)C>[ClH:12].[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH:10]([OH:13])[CH2:11][NH:16][CH2:14][CH3:15])=[CH:4][C:3]=2[O:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6341EthylamineHCID 224917731-(3,4-Methylenedioxyphenyl)-2-chloroethanol

生成物 1

HCID 213260981-(3,4-Methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

19.5 g. of 1-(3,4-methylenedioxyphenyl)-2-chloroethanol are added to a solution of 170 g. of ethylamine in 200 ml. of cooled ethanol and the mixture is heated at 80° C. for 8 hours in an autoclave. After cooling, the ethanol and excess ethylamine are distilled off under reduced pressure. The residue is extracted with 100 ml. of 1N HCl and the extract is washed twice with 100 ml. of ether. The hydrochloric acid extract solution is made basic with 1N caustic soda and the liberated oil is extracted with ether. The ether extract is dried and an etherial hydrochloric acid solution is added thereto. The crystals which settle out on standing are filtered off and washed with ether. Upon recrystallization from isopropyl alcohol 7.8 g. of 1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride are obtained.

後処理

  1. temperatureAfter cooling
  2. distillationthe ethanol and excess ethylamine are distilled off under reduced pressure
  3. extractionThe residue is extracted with 100 ml
  4. washof 1N HCl and the extract is washed twice with 100 ml
  5. extractionThe hydrochloric acid extract solution
  6. extractionthe liberated oil is extracted with ether
  7. extractionThe ether extract
  8. customis dried
  9. additionan etherial hydrochloric acid solution is added
  10. filtrationare filtered off
  11. washwashed with ether
  12. customUpon recrystallization from isopropyl alcohol 7.8 g

出典と根拠

ORDレコード
ord-bc4afb999e334a7e83a6e8b4148ff609
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04147799

反応ノート

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