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

Sulfuric Acid → 4-(4-Bromophenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline

HRID 1072507
ノート
印刷プレビュー

反応式

HRID 1072507 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8](O)[CH2:9][N:10]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[Cl:20])[CH3:11])=[CH:4][CH:3]=1.OS(O)(=O)=O.[OH-].[Na+]>ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:18]3[C:13](=[C:14]([Cl:20])[CH:15]=[C:16]([Cl:19])[CH:17]=3)[CH2:12][N:10]([CH3:11])[CH2:9]2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 223868482-((2,4-Dichlorobenzyl)(methyl)amino)-1-(4-bromophenyl)ethanol

生成物 1

HCID 101772114-(4-Bromophenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5.45 g (14.0 mmol) of 1-(4-bromo-phenyl)-2-[(2,4-dichloro-benzyl)-methyl-amino]-ethanol was introduced into 15 ml of dichloromethane and, at 0° C., 15 ml of conc. H2SO4 are added. After stirring at room temperature for 2 hours, the reaction mixture was poured onto ice and made alkaline with 6 N NaOH. Three extractions with dichloromethane were carried out. The combined organic phases were dried with MgSO4 and concentrated. For further purification, the residue was chromatographed on silica gel, resulting in 2.6 g of the title compound as a yellowish oil. 4-(4-Bromo-phenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline, Hydrochloride;

後処理

  1. additionthe reaction mixture was poured onto ice
  2. extractionThree extractions with dichloromethane
  3. dry with materialThe combined organic phases were dried with MgSO4
  4. concentrationconcentrated
  5. customFor further purification
  6. customthe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-e8bff8e7970649649270640a359d5372
出典データセット
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06911453B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート