Hydrochloric Acid → alpha-(3,4-Dimethoxyphenethylaminomethyl)-2-methoxybenzylalcohol hydrochloride

HRID 66320노트

반응식

HRID 66320 반응식
[Cl:1][CH2:2][CH:3]([OH:12])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][CH3:11].[CH3:13][O:14][C:15]1[CH:16]=[C:17]([CH:21]=[CH:22][C:23]=1[O:24][CH3:25])[CH2:18][CH2:19][NH2:20].C(Cl)(Cl)Cl.Cl>C(O)C.C(OCC)C>[ClH:1].[CH3:13][O:14][C:15]1[CH:16]=[C:17]([CH:21]=[CH:22][C:23]=1[O:24][CH3:25])[CH2:18][CH2:19][NH:20][CH2:2][CH:3]([OH:12])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][CH3:11]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 8421HomoveratrylamineHCID 224917592-Chloro-1-(2-methoxyphenyl)ethan-1-ol

생성물 1

HCID 22754925alpha-(3,4-Dimethoxyphenethylaminomethyl)-2-methoxybenzylalcohol hydrochloride수율 41.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

A mixture of 3.7 g of α-chloromethyl-2-methoxybenzylalcohol (crude oil) and 10.9 g of 3,4-dimethoxyphenethylamine is heated at 130° to 140° C. for 2 hours. After cooling, chloroform is added to the reaction mixture, and said mixture is washed with water. The mixture is dried and evaporated to remove solvent. 30 ml of ethanol are added to the residue obtained. Then, hydrochloric acid-containing diethylether is added to the ethanol mixture, and crystalline precipitates are collected by filtration. 3.0 g of α-(3,4-dimethoxyphenethylaminomethyl)-2-methoxybenzylalcohol hydrochloride are obtained as crystals. M.p. 142°-143° C.

후처리

  1. temperatureis heated at 130° to 140° C. for 2 hours
  2. temperatureAfter cooling
  3. washis washed with water
  4. customThe mixture is dried
  5. customevaporated
  6. customto remove solvent
  7. addition30 ml of ethanol are added to the residue
  8. customobtained
  9. customcrystalline precipitates
  10. filtrationare collected by filtration

출처 및 근거

ORD 기록
ord-fe01ba9c7d884a63b445b6e999ea679e
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04131686

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