ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Triethylamine → HCID 13579648、化合物

HRID 1380880
ノート
印刷プレビュー

反応式

HRID 1380880 の反応式
[CH3:1][NH:2][CH:3]1[CH2:12][CH2:11][C:10]2[C:5](=[CH:6][C:7]([O:15][CH3:16])=[C:8]([O:13][CH3:14])[CH:9]=2)[CH2:4]1.C(N(CC)CC)C.[CH3:24][O:25][C:26]1[C:41]([O:42][CH3:43])=[CH:40][C:29]2[CH2:30][C:31](=[O:39])[N:32]([CH2:35][CH2:36][CH2:37]Cl)[CH:33]=[CH:34][C:28]=2[CH:27]=1>[OH-].[Na+].C(OCC)(=O)C>[CH3:24][O:25][C:26]1[C:41]([O:42][CH3:43])=[CH:40][C:29]2[CH2:30][C:31](=[O:39])[N:32]([CH2:35][CH2:36][CH2:37][N:2]([CH3:1])[CH:3]3[CH2:12][CH2:11][C:10]4[C:5](=[CH:6][C:7]([O:15][CH3:16])=[C:8]([O:13][CH3:14])[CH:9]=4)[CH2:4]3)[CH:33]=[CH:34][C:28]=2[CH:27]=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 12381618HCID 12381618、化合物HCID 130925033-(3-Chloropropyl)-1,3-dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one

生成物 1

HCID 13579648HCID 13579648、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 14798Sodium Hydroxide溶媒

反応条件

温度
90 °C

実験手順

A mixture of 2-methylamino-6,7-dimethoxy-1,2,3,4-tetrahydronaphthalene (1.72 g, 0.0078 mol), triethylamine (1.09 ml, 0.0078 mol) and 1-(7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-on-3-yl)-3-chloropropane (2.3 g, 0.0078 mol) is heated to a reaction temperature of 90° C. in steps within one hour and kept at this temperature for 2 hours. The initial suspension slowly changes into a clear solution and begins to precipitate in a jelly-like manner after about 30 minutes. The cooled reaction mixture is dissolved in 0.5M sodium hydroxide solution/ethyl acetate, the organic phase is washed with water, dried over magnesium sulphate, concentrated by evaporation in vacuo and purified over alumina (300 g), neutral, activity II, with methylene chloride and then with increasing quantities of ethanol (up to 20%). The hydrochloride is precipitated from a solution in acetone using ethereal hydrochloric acid. Yield: 1.39 g Mp: >125° C. (Decomp.).

後処理

  1. customto precipitate in a jelly-like manner after about 30 minutes
  2. customThe cooled reaction mixture
  3. washthe organic phase is washed with water
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated by evaporation in vacuo
  6. custompurified over alumina (300 g)
  7. customThe hydrochloride is precipitated from a solution in acetone using ethereal hydrochloric acid

出典と根拠

ORDレコード
ord-cf0c2551ba97461b94639a562ffeb1a7
出典データセット
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04584293

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