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Diisopropylethylamine → [4-({[2-(Benzo[1,3]dioxol-5-yloxy)-pyridine-3-carbonyl]-amino}-methyl)-phenyl]-acetic acid methyl ester

HRID 1297582
ノート
印刷プレビュー

反応式

HRID 1297582 の反応式
Cl.CN(C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1.[O:24]1[C:28]2[CH:29]=[CH:30][C:31]([O:33][C:34]3[N:42]=[CH:41][CH:40]=[CH:39][C:35]=3[C:36]([OH:38])=O)=[CH:32][C:27]=2[O:26][CH2:25]1.C(N(CC)C(C)C)(C)C.[CH3:52][O:53][C:54](=[O:64])[CH2:55][C:56]1[CH:61]=[CH:60][C:59]([CH2:62][NH2:63])=[CH:58][CH:57]=1>ClCCl.O>[CH3:52][O:53][C:54](=[O:64])[CH2:55][C:56]1[CH:61]=[CH:60][C:59]([CH2:62][NH:63][C:36]([C:35]2[C:34]([O:33][C:31]3[CH:30]=[CH:29][C:28]4[O:24][CH2:25][O:26][C:27]=4[CH:32]=3)=[N:42][CH:41]=[CH:40][CH:39]=2)=[O:38])=[CH:58][CH:57]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 81531DiisopropylethylamineHCID 1514145Methyl 4-aminomethylphenylacetateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27368792-(1,3-Benzodioxol-5-yloxy)pyridine-3-carboxylic acidHCID 27960291-Hydroxybenzotriazole hydrate

生成物 1

HCID 10202284
[4-({[2-(Benzo[1,3]dioxol-5-yloxy)-pyridine-3-carbonyl]-amino}-methyl)-phenyl]-acetic acid methyl ester

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

1-[3-(Dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (1.71 g), 1-hydoxybenzo-triazole hydrate (1.24 g), and 2-(benzo[1,3]dioxol-5-yloxy)-nicotinic acid were combined and suspended in anhydrous dichloromethane (40 mL). N,N-diisopropylethylamine (5.93 mL) was added to the suspension, which was stirred for 0.5 h. The suspension was added to (4-aminomethyl-phenyl)-acetic acid methyl ester (1.22 g) and the reaction mixture stirred at ambient temperature overnight. Water (approx. 15 mL) was then added to the reaction mixture, and it was extracted with dichloromethane (7×30 mL). The combined organics were dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude product was purified by silica gel chromatography (ethyl acetate:hexanes=3:2) to yield the title compound (1.41 g).

後処理

  1. stirringthe reaction mixture stirred at ambient temperature overnight
  2. extractionwas extracted with dichloromethane (7×30 mL)
  3. dry with materialThe combined organics were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by silica gel chromatography (ethyl acetate:hexanes=3:2)

出典と根拠

ORDレコード
ord-2fb9f61ea113439fbf08775257eedea3
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07250518B2

反応ノート

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