Hydrochloric Acid → HCID 20431221、化合物

HRID 2412850

反応式

HRID 2412850 の反応式
[ClH:1].[CH3:2][CH:3]1[O:8][CH:7]([CH3:9])[CH2:6][NH:5][CH2:4]1.[C:10]([C:14]1[CH:19]=[CH:18][C:17]([C:20](=[O:23])[CH2:21][CH3:22])=[CH:16][CH:15]=1)([CH3:13])([CH3:12])[CH3:11].[CH2:24]=O.Cl>C(O)C>[ClH:1].[C:10]([C:14]1[CH:15]=[CH:16][C:17]([C:20](=[O:23])[CH:21]([CH3:24])[CH2:22][N:5]2[CH2:6][CH:7]([CH3:9])[O:8][CH:3]([CH3:2])[CH2:4]2)=[CH:18][CH:19]=1)([CH3:13])([CH3:12])[CH3:11]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 5952814'-(tert-Butyl)propiophenoneHCID 19374754HCID 19374754、化合物

生成物 1

HCID 20431221HCID 20431221、化合物収率 30%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

57.6 g (0.5 mole) of 2,6-dimethylmorpholine hydrochloride, 95.2 g (0.5 mole) of p-tert.-butyl-propiophenone and 25 g (0.83 mole) of paraformaldehyde were heated under reflux in 200 ml of ethanol for 1 hour. After adding 0.7 ml of concentrated hydrochloric acid, the reaction mixture was stirred under reflux for a further 15 hours. It was then concentrated, the residue was taken up in chloroform and the chloroform mixture was washed twice with water, dried over sodium sulphate and concentrated. The solid residue was suspended in hot ethyl acetate, filtered off and dried. 47.6 g (30% of theory) of p-tert.-butyl-2-methyl-3-(2,6-dimethylmorpholin-4yl)-propionphenone hydrochloride were obtained and were dissolved in aqueous sodium bicarbonate solution and the solution and 25 g (0.83 mole) of paraformaldehyde were heated under reflux in 200 ml of ethanol for 1 hour. After adding 0.7 ml of concentrated hydrochloric acid, the reaction mixture was stirred under reflux for a further 15 hours. It was then concentrated, the residue was taken up in chloroform and the chloroform mixture was washed twice with water, dried over sodium sulphate and concentrated. The solid residue was suspended in hot ethyl acetate, filtered off and dried. 47.6 g (30% of theory) of p-tert.-butyl-2-methyl-3-(2,6-dimethylmorpholin-4yl)-propionphenone hydrochloride were obtained and were dissolved in aqueous sodium bicarbonate solution and the solution was then extracted with ethyl acetate and the product phase concentrated. A quantative yield of the free base of boiling point 145°-48° C./0.12 mm Hg column was obtained. ##STR59##

後処理

  1. temperatureunder reflux for a further 15 hours
  2. concentrationIt was then concentrated
  3. washthe chloroform mixture was washed twice with water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated
  6. filtrationfiltered off
  7. customdried

出典と根拠

ORDレコード
ord-c551a54059394019a83b0b00aa5a94ca
出典データセット
uspto-grants-1985_01
特許番号
US04495184

関連ノート

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