Hydrochloric Acid → HCID 12842152, 화합물

HRID 435111

반응식

HRID 435111 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 12842152HCID 12842152, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5f831d5144b6416ea3bb99e62c3f634f
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04400380

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