Hydrochloric Acid → HCID 70507303, 화합물

HRID 358213

반응식

HRID 358213 반응식
[ClH:1].[NH:2]1[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.[C:8]([C:12]1[CH:17]=[CH:16][C:15]([C:18](=[O:21])[CH2:19][CH3:20])=[CH:14][CH:13]=1)([CH3:11])([CH3:10])[CH3:9].[CH2:22]=O.Cl>C(O)C>[ClH:1].[C:8]([C:12]1[CH:13]=[CH:14][C:15]([C:18](=[O:21])[CH:19]([CH3:22])[CH2:20][N:2]2[CH2:7][CH2:6][O:5][CH2:4][CH2:3]2)=[CH:16][CH:17]=1)([CH3:11])([CH3:10])[CH3:9]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 197884Morpholine, hydrochloride (1:1)HCID 5952814'-(tert-Butyl)propiophenone

생성물 1

HCID 70507303HCID 70507303, 화합물수율 61.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

37.07 g (0.3 mole) of morpholine hydrochloride, 57.1 g (0.3 mole) of p-tert.-butyl-propiophenone and 15.01 g (0.5 mole) of paraformaldehyde were heated under reflux in 150 ml of ethanol for 1 hour. After adding 0.5 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, the chloroform mixture was washed twice with water and the organic phase was dried over sodium sulphate and concentrated. The crystalline residue was suspended in hot ethyl acetate, filtered off and dried. 60 g (61.5% of theory) of p-tert.-butyl-2-methyl-3-morpholin-4-yl-propiophenone hydrochloride of melting point 189° to 91° C. were obtained.

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 materialthe organic phase was dried over sodium sulphate
  5. concentrationconcentrated
  6. filtrationfiltered off
  7. customdried

출처 및 근거

ORD 기록
ord-62a2654f9dba4e319efe497df3f64a86
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04465678

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