HCID 20517506, 화합물 → HCID 20517553, 화합물

HRID 2198890노트

반응식

HRID 2198890 반응식
[CH2:1]([C:3]1([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16]C)[CH:11]=2)[O:8][CH:7]([CH3:9])[CH2:6][NH:5][CH2:4]1)[CH3:2]>Br>[CH2:1]([C:3]1([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([OH:16])[CH:11]=2)[O:8][CH:7]([CH3:9])[CH2:6][NH:5][CH2:4]1)[CH3:2]

참가 물질

3

반응물 1

HCID 20517506HCID 20517506, 화합물

생성물 1

HCID 20517553HCID 20517553, 화합물수율 113.2%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

2-Ethyl-2-(3-methoxyphenyl)-6-methylmorpholine (2.63 g) was refluxed with aq 48% HBr (20 ml) for 2.5 h. The residue on evaporation was re-evaporated from isopropyl alcohol several times, giving ultimately a green gum (2.8 g), which was dissolved in methanol and basified with 0.880 ammonia. The methanol and ammonia were evaporated under reduced pressure and the aqueous remaining was shaken with chloroform (2×100 ml). The chloroform layers were washed and dried and evaporated, leaving an orange oil (8.4 g) that crystallised from ethyl acetate (25 ml). The yellow hygroscopic solid was dissolved in isopropyl alcohol (15 ml) and acidified with ethereal hydrogen chloride. On cooling crystals of the title compound hydrochloride were obtained (0.85 g, mp 200°-205° C.). Gas-liquid chromatography revealed the isomer ratio to be 20:1.

후처리

  1. customThe residue on evaporation
  2. customwas re-evaporated from isopropyl alcohol several times

출처 및 근거

ORD 기록
ord-fc64a721cf4d4f86a2719c32c15f668f
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04360519

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