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Methyl 2-[(2-methoxyethoxy)methoxy]-3-(5-methoxypyridin-2-ylamino)benzoate → Methyl-2-hydroxy-3-(5-methoxypyridin-2-ylamino)benzoate

HRID 912431
ノート
印刷プレビュー

反応式

HRID 912431 の反応式
COCCOC[O:7][C:8]1[C:17]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][N:20]=2)=[CH:16][CH:15]=[CH:14][C:9]=1[C:10]([O:12][CH3:13])=[O:11]>CO>[CH3:13][O:12][C:10](=[O:11])[C:9]1[CH:14]=[CH:15][CH:16]=[C:17]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][N:20]=2)[C:8]=1[OH:7]
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

3

反応物 1

HCID 67410020Methyl 2-[(2-methoxyethoxy)methoxy]-3-(5-methoxypyridin-2-ylamino)benzoate

生成物 1

HCID 67410207Methyl-2-hydroxy-3-(5-methoxypyridin-2-ylamino)benzoate収率 91.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
40 °C

実験手順

To a solution of methyl 2-[(2-methoxyethoxy)methoxy]-3-(5-methoxypyridin-2-ylamino)benzoate 1.0 g (2.8 mmol) of step 3 in methanol 20 mL was added 6NHCl 2 mL, followed by stirring at 40° C. for 30 min. The reaction mixture was cooled to room temperature, concentrated in a vacuum, diluted with ethylacetate, washed with distilled water, and a saturated NaCl solution. After drying over magnesium sulfate and concentration in a vacuum, purification by column chromatography (developing solvent: ethylacetate/hexane=1/2) afforded 0.70 g of the title compound (yield 90%).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated in a vacuum
  3. additiondiluted with ethylacetate
  4. washwashed with distilled water
  5. dry with materialAfter drying over magnesium sulfate and concentration in a vacuum, purification by column chromatography (developing solvent: ethylacetate/hexane=1/2)

出典と根拠

ORDレコード
ord-a95e4aae34fc43d6b0bfc6872a39ac81
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08026235B1

反応ノート

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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