Hydrochloric Acid → HCID 20431221, 화합물

HRID 2412850

반응식

HRID 2412850 반응식
[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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 5952814'-(tert-Butyl)propiophenoneHCID 19374754HCID 19374754, 화합물

생성물 1

HCID 20431221HCID 20431221, 화합물수율 30%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-c551a54059394019a83b0b00aa5a94ca
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04495184

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