Hydrochloric Acid → HCID 12842152、化合物

HRID 435111

反応式

HRID 435111 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]=[CH:9][C:10](=[O:12])[CH3:11])=[CH:4][CH:3]=1.[CH2:13]=O.[NH:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1.[ClH:21]>C(O)C.CC(C)=O>[ClH:21].[CH3:1][C:2]1[CH:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10](=[O:12])[CH2:11][CH2:13][N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 8083MorpholineHCID 1073884-(4-Methylphenyl)-3-buten-2-one

生成物 1

HCID 12842152HCID 12842152、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 702Ethanol溶媒

実験手順

8 g (0.05 mole) of 4-(4-methylphenyl)-3-buten-2-one (prepared analogously to the intermediates for the foregoing examples), 2 g (a 30% excess) of paraformaldehyde and 4.35 g (0.05 mole) of morpholine are dissolved in a mixture of ethanol (60 ml) and concentrated HCl (6 ml). The mixture is heated at reflux temperature for 18 hours. The mixture is then cooled to room temperature and diluted with acetone to a volume of 250 ml. The solution is chilled overnight. It is then concentrated to a volume of about 25 ml. The residue is triturated with ethyl alcohol. The insoluble material is filtered and recrystallized from ethyl alcohol/methyl alcohol. The resultant crystals are filtered and vacuum dried overnight, yielding 3.3 g of (E)-1-(4-methylphenyl)-5-(4-morpholinyl)-1-penten-3-one hydrochloride; m.p. 188°-190° C.

後処理

  1. temperatureThe mixture is heated
  2. temperatureat reflux temperature for 18 hours
  3. temperatureThe solution is chilled overnight
  4. concentrationIt is then concentrated to a volume of about 25 ml
  5. customThe residue is triturated with ethyl alcohol
  6. filtrationThe insoluble material is filtered
  7. customrecrystallized from ethyl alcohol/methyl alcohol
  8. filtrationThe resultant crystals are filtered
  9. customvacuum dried overnight

出典と根拠

ORDレコード
ord-5f831d5144b6416ea3bb99e62c3f634f
出典データセット
uspto-grants-1983_08
特許番号
US04400380

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