HCID 20517506、化合物 → HCID 20517553、化合物

HRID 2198890ノート

反応式

HRID 2198890 の反応式
[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]

参加物

3

反応物 1

HCID 20517506HCID 20517506、化合物

生成物 1

HCID 20517553HCID 20517553、化合物収率 113.2%

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-fc64a721cf4d4f86a2719c32c15f668f
出典データセット
uspto-grants-1982_11
特許番号
US04360519

反応ノート

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