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Sodium hydride → methyl 2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylate

HRID 840300
ノート
印刷プレビュー

反応式

HRID 840300 の反応式
[CH2:1]([NH:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][N:5]=1)[CH3:2].[H-].[Na+].[CH2:16]([O:23][C:24]1[CH:31]=[CH:30][C:29]([Br:32])=[CH:28][C:25]=1[CH2:26]Br)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>CN(C=O)C>[CH3:11][O:10][C:8]([C:7]1[CH:12]=[CH:13][C:4]([N:3]([CH2:26][C:25]2[CH:28]=[C:29]([Br:32])[CH:30]=[CH:31][C:24]=2[O:23][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:1][CH3:2])=[N:5][CH:6]=1)=[O:9]
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 24758Sodium hydrideHCID 11126856Methyl 6-(ethylamino)pyridine-3-carboxylateHCID 117832201-(Benzyloxy)-4-bromo-2-(bromomethyl)benzene

生成物 1

HCID 22622546methyl 2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylate収率 71%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of methyl 6-ethylaminonicotinoate (15.2 g, 84.4 mmol) in DMF (50 ml) was cooled to 0 ° C. and treated with sodium hydride (60%, 75 mmol). The reaction was stirred for 1 hour and a solution of 2-benzyloxy-5-bromobenzylbromide (25 g, 70.2 mmol) in DMF (50 ml) added. The reaction was allowed to warm to ambient temperature and stirred for 18 hours. The reaction was quenched with water and extracted with ethyl acetate (three times). The organic layers were combined, washed with water and brine twice, dried (MgSO4) and evaporated to give a white solid. Recrystallisation from ethyl acetate/hexane gave methyl-2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylate (22.7 g, 71%).

後処理

  1. stirringstirred for 18 hours
  2. customThe reaction was quenched with water
  3. extractionextracted with ethyl acetate (three times)
  4. washwashed with water and brine twice
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto give a white solid
  8. customRecrystallisation from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-f0fda7f9849b47e8a01071e6e8bca003
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06365603B1

反応ノート

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