Methanol → 1-Methyl-3-phenoxypropyldiethylamine

HRID 484833ノート

反応式

HRID 484833 の反応式
CO.S(C1C=CC(C)=CC=1)(O[CH:7]([CH2:9][CH2:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH3:8])(=O)=O.[CH2:25]([NH:27][CH2:28][CH3:29])[CH3:26].C(OCC)C>C(Cl)(Cl)Cl>[CH3:8][CH:7]([N:27]([CH2:28][CH3:29])[CH2:25][CH3:26])[CH2:9][CH2:10][O:11][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

6

反応物 4

HCID 887MethanolHCID 3283Diethyl EtherHCID 8021DiethylamineHCID 133267624-Phenoxy-2-butyl tosylate

生成物 1

HCID 135201021-Methyl-3-phenoxypropyldiethylamine収率 77%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To 60 ml of absolute methyl alcohol were added 10 g of 4-phenoxy-2-butyl tosylate and 9.62 g of diethylamine. The mixture was reacted in a sealed tube for one hour at 125° C. After the reaction solution was condensed under reduced pressure, 100 ml of diethyl ether was added into the solution, and then the solution was separated into the diethyl ether solution and 20% aqueous sodium hydroxide solution. The ether layer was dried over anhydrous sodium sulfate, and the ether was removed under reduced pressure therefrom. The residue thus obtained was subjected to an alumina-column chromatography using chloroform as the developing solvent to give 5.32 g of 1-methyl-3-phenoxypropyldiethylamine in a yield of 77%.

後処理

  1. customThe mixture was reacted in a sealed tube for one hour at 125° C
  2. additionwas added into the solution
  3. customthe solution was separated into the diethyl ether solution and 20% aqueous sodium hydroxide solution
  4. dry with materialThe ether layer was dried over anhydrous sodium sulfate
  5. customthe ether was removed under reduced pressure
  6. customThe residue thus obtained

出典と根拠

ORDレコード
ord-0860664dcb4b40f994a1eef0f1399a4b
出典データセット
uspto-grants-1985_08
特許番号
US04533731

反応ノート

読み込み中…