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Morpholine → 2,3-Dihydro-4-methyl-2-[2-(4-morpholinyl)ethyl]pyrido[3,2-f][1,4]oxazepin-5(4H)-thione

HRID 236184
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반응식

HRID 236184 반응식
Cl[CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH3:11])[C:8](=[S:12])[C:7]2[CH:13]=[CH:14][CH:15]=[N:16][C:6]=2[O:5]1.[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1>>[CH3:11][N:9]1[C:8](=[S:12])[C:7]2[CH:13]=[CH:14][CH:15]=[N:16][C:6]=2[O:5][CH:4]([CH2:3][CH2:2][N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[CH2:10]1
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참가 물질

3

반응물 2

HCID 8083MorpholineHCID 137264422-(chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f]-1,4-oxazepine-5(4H)thione

생성물 1

HCID 137264902,3-Dihydro-4-methyl-2-[2-(4-morpholinyl)ethyl]pyrido[3,2-f][1,4]oxazepin-5(4H)-thione

실험 절차

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepine-5(4H)-thione, 4.5 g (0.018 mole) was dissolved in morpholine (30 ml). The solution was heated with stirring to 50°-60° C. for 6 hr. The morpholine was then removed by rotary evaporation (90° C., vacuum pump). The residue was taken up in chloroform (100 ml) and washed with dilute aqueous sodium hydroxide (2×30 ml). The organic layer was concentrated by rotary evaporation (60° C., water aspirator). The residue was recrystallized from ethanol giving 3.26 g (60%) of light yellow crystals, m.p. 152°-153° C.

후처리

  1. temperatureThe solution was heated
  • customThe morpholine was then removed by rotary evaporation (90° C., vacuum pump)
  • washwashed with dilute aqueous sodium hydroxide (2×30 ml)
  • concentrationThe organic layer was concentrated by rotary evaporation (60° C., water aspirator)
  • customThe residue was recrystallized from ethanol giving 3.26 g (60%) of light yellow crystals, m.p. 152°-153° C.
  • 출처 및 근거

    ORD 기록
    ord-28c70d228ee744c58538dfd3cc0569e9
    출처 데이터셋
    uspto-grants-1987_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04642343

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