Hydrochloric Acid → HCID 70507303、化合物

HRID 358213

反応式

HRID 358213 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 70507303HCID 70507303、化合物収率 61.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

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

出典と根拠

ORDレコード
ord-62a2654f9dba4e319efe497df3f64a86
出典データセット
uspto-grants-1984_08
特許番号
US04465678

関連ノート

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