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Methylamine → (3-Methoxy)-alpha-methyl-alpha-[(methylamino)methyl]benzene methanol

HRID 2198883
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반응식

HRID 2198883 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9]2([CH3:12])[CH2:11][O:10]2)[CH:6]=[CH:7][CH:8]=1.[CH3:13][NH2:14]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9]([CH3:12])([CH2:11][NH:14][CH3:13])[OH:10])[CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6329Methylamine2회HCID 204969162-(3-Methoxyphenyl)-2-methyloxirane

생성물 1

HCID 62773765(3-Methoxy)-alpha-methyl-alpha-[(methylamino)methyl]benzene methanol

실험 절차

2-(3-Methoxyphenyl)-2-methyloxiran (34.0 g) was stirred with aqueous methylamine (100 ml, 33%) and alcoholic methylamine (200 ml, 33%) overnight at ambient temperature. The mixture was evaporated to an oil under reduced pressure, dissolved in hydrochloric acid (2 M) and extracted with toluene. After basifying the aqueous acid with sodium hydroxide (5 M) the basic oil was extracted with toluene and dried (MgSO4). The solvent was removed under reduced pressure to leave the title compound as an oil (27.7 g). The hydrochloride was formed in isopropyl alcohol-ethereal hydrogen chloride, m.p. 155°-156° C. (Found: C, 57.55; H, 8.3; N, 5.8% C11H17NO2HCl requires C, 57.0; H, 7.8; N, 6.0%.

후처리

  1. customThe mixture was evaporated to an oil under reduced pressure
  • dissolutiondissolved in hydrochloric acid (2 M)
  • extractionextracted with toluene
  • extractionwas extracted with toluene
  • dry with materialdried (MgSO4)
  • customThe solvent was removed under reduced pressure
  • 출처 및 근거

    ORD 기록
    ord-51f1fa9dfe4c4beaa34acf22188b01d7
    출처 데이터셋
    uspto-grants-1982_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04360519

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