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

HRID 26002
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HRID 26002 반응식
[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
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bc4afb999e334a7e83a6e8b4148ff609
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04147799

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