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

HRID 66320ノート

反応式

HRID 66320 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fe01ba9c7d884a63b445b6e999ea679e
出典データセット
uspto-grants-1978_12
特許番号
US04131686

反応ノート

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