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

HRID 1455969
ノート
印刷プレビュー

反応式

HRID 1455969 の反応式
[H-].[Na+].[CH2:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([O:14][CH3:15])=[O:13])=[CH:8][N:7]=1)[CH3:4].[Br:16][C:17]1[CH:18]=[CH:19][C:20]([O:25][CH2:26][C:27]2[S:28][CH:29]=[CH:30][CH:31]=2)=[C:21]([CH:24]=1)[CH2:22]Br.[Cl-].[NH4+]>CN(C=O)C>[S:28]1[CH:29]=[CH:30][CH:31]=[C:27]1[CH2:26][O:25][C:20]1[CH:19]=[CH:18][C:17]([Br:16])=[CH:24][C:21]=1[CH2:22][N:5]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([O:14][CH3:15])=[O:13])=[CH:8][N:7]=1)[CH2:3][CH3:4]
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 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 11126856Methyl 6-(ethylamino)pyridine-3-carboxylateHCID 221055055-Bromo-2-(2-thienylmethoxy)benzyl bromide

生成物 1

HCID 22105529methyl 2-[N-(2-(2-thienylmethoxy)-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylate収率 8.1%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
2 回

反応条件

温度
-5 °C

実験手順

A suspension of sodium hydride (50% dispersion 0.8 mmol, 38 mg) in DMF (2 ml) (sieve dried) was cooled to -5° C. and treated with methyl 2-(ethylamino)pyridine-5-carboxylate (0.145 g, 0.8 mmol). The reaction was stirred at -5° C. for 30 minutes and then treated with 5-bromo-2-(2-thienylmethoxy)benzyl bromide (0.29 g, 0.8 mmol) in DMF (0.5 ml). The reaction was allowed to warm to ambient temperature and stirred for 18 hours. The reaction was poured into saturated aqueous ammonium chloride. The combined organic extracts were washed once with brine, dried (MgSO4) and evaporated. The residue was purified by chromatography (eluant: diethyl ether/hexane) to give methyl 2-[N-(2-(2-thienylmethoxy)-5-bromobenzyl)N-ethylamino]pyridine-5-carboxylate as a colourless oil (0.03 g, 8%).

後処理

  1. temperatureto warm to ambient temperature
  2. stirringstirred for 18 hours
  3. washThe combined organic extracts were washed once with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe residue was purified by chromatography (eluant: diethyl ether/hexane)

出典と根拠

ORDレコード
ord-90b2519442f947878d9920ee3e4fb4f7
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05843942

反応ノート

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