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Triethylamine → HCID 13319934、化合物

HRID 1154682
ノート
印刷プレビュー

反応式

HRID 1154682 の反応式
[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][Cl:15])[CH2:10][CH2:11][C:5]=2[CH:4]=1.C(N(CC)CC)C.[CH3:28][NH:29][CH2:30][CH2:31][CH2:32][C:33]1[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[C:35]([O:41][CH3:42])[CH:34]=1>C(Cl)Cl.O.CC(C)=O>[ClH:15].[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][N:29]([CH3:28])[CH2:30][CH2:31][CH2:32][C:33]3[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[C:35]([O:41][CH3:42])[CH:34]=3)[CH2:10][CH2:11][C:5]=2[CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 7131256N-[3-(3,4-dimethoxyphenyl)propyl]-N-methylamineHCID 130925103-(3-Chloropropyl)-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one

生成物 1

HCID 13319934HCID 13319934、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 21908982
Water methylene chloride
溶媒

反応条件

温度
85 °C

実験手順

A mixture of 5.55 gm (0.0186 mol) of 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-chloro-propane, 2.6 ml (0.0886 mol) of triethylamine and 3.9 gm (0.0186 mol) of N-methyl-3-(3,4-dimethoxy-phenyl) propylamine was heated at 85° C. for 4 hours, then cooled and dissolved in methylene chloride/water. The organic phase was separated, extracted with water, dried over magnesium sulfate, concentrated by evaporation in vacuo, and the residue was purified on silica gel, using methylene chloride plus 3% ethanol as the eluant. The oily free base product thus obtained was dissolved in acetone, and the hydrochloride was precipitated with ethereal hydrochloric acid.

後処理

  1. temperaturecooled
  2. customThe organic phase was separated
  3. extractionextracted with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated by evaporation in vacuo
  6. customthe residue was purified on silica gel
  7. customThe oily free base product thus obtained
  8. customthe hydrochloride was precipitated with ethereal hydrochloric acid

出典と根拠

ORDレコード
ord-74f942d0bc2243a392b182cd56219b63
出典データセット
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04490369

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート