Methylamine → HCID 20186775、化合物

HRID 2309008ノート

反応式

HRID 2309008 の反応式
[C:1]([CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH:14]([NH:16][CH2:17][CH:18]([O:26][CH2:27][CH2:28][OH:29])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)[CH3:15])=[CH:9][CH:8]=1)(OC)=[O:2].[CH3:30][NH2:31]>C(O)C>[ClH:25].[CH3:30][NH:31][C:1]([CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH:14]([NH:16][CH2:17][CH:18]([O:26][CH2:27][CH2:28][OH:29])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)[CH3:15])=[CH:9][CH:8]=1)=[O:2]

参加物

4

反応物 2

HCID 6329MethylamineHCID 21285459HCID 21285459、化合物

生成物 1

HCID 20186775HCID 20186775、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of N-[2-(4-carbomethoxymethoxyphenyl)-1-methylethyl]-2-(2-hydroxyethoxy)-2-(3-chlorophenyl)ethanamine (4.0 g) and 33% methylamine in ethanol (50 ml) was heated under reflux for 1.5 h. The mixture was evaporated under reduced pressure and the residue converted to its hydrochloride by addition of ethereal hydrogen chloride. Recrystallisation from ethyl acetate-methanol gave the title compound, mp. 117°-121° C. as a 56:44 mixture of diastereoisomers.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1.5 h
  3. customThe mixture was evaporated under reduced pressure
  4. additionthe residue converted to its hydrochloride by addition of ethereal hydrogen chloride
  5. customRecrystallisation from ethyl acetate-methanol

出典と根拠

ORDレコード
ord-a3d7d059f30744e193bf503e17563581
出典データセット
uspto-grants-1987_09
特許番号
US04692465

反応ノート

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