Water → 2-{[3-Methoxy-4-(2-thiophene-2-ylvinyl)phenyl]methylamino}ethanol

HRID 85311ノート

反応式

HRID 85311 の反応式
[OH-].[Na+].O.[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH2:19][NH:20][CH2:21][CH2:22][O:23]C(=O)C(C)(C)C)[CH:9]=[CH:10][C:11]=1[CH:12]=[CH:13][C:14]1[S:15][CH:16]=[CH:17][CH:18]=1>C(O)C>[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH2:19][NH:20][CH2:21][CH2:22][OH:23])[CH:9]=[CH:10][C:11]=1[CH:12]=[CH:13][C:14]1[S:15][CH:16]=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 68008944HCID 68008944、化合物

生成物 1

HCID 680089612-{[3-Methoxy-4-(2-thiophene-2-ylvinyl)phenyl]methylamino}ethanol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
45 °C

実験手順

NaOH (4.3 g, 107 mmol) was dissolved in ethanol (25 ml), and water (7 ml) was added thereto. Next, 2,2-dimethylpropionic acid 2-{[3-methoxy-4-(2-thiophene-2-ylvinyl)phenyl]methylamino}ethyl ester (4.0 g, 10.7 mmol) was dissolved in ethanol (8 ml) and added dropwise to the mixture. The mixture was stirred at room temperature for 2 hours and further at 45° C. for 1 hour. After the solvent was evaporated off, water (100 ml) was added and the oily matter was subjected to extraction with ethyl acetate. After 2 times of washing with water, drying over Na2SO4 and concentration were performed. The residue was purified by silica gel chromatography to give a yellow oily matter (yield: 3.1 g (100%)).

後処理

  1. additionadded dropwise to the mixture
  2. customAfter the solvent was evaporated off
  3. additionwater (100 ml) was added
  4. extractionthe oily matter was subjected to extraction with ethyl acetate
  5. washAfter 2 times of washing with water
  6. dry with materialdrying over Na2SO4 and concentration
  7. customThe residue was purified by silica gel chromatography
  8. customto give a yellow oily matter (yield: 3.1 g (100%))

出典と根拠

ORDレコード
ord-46f212c4d6a142638df8ed39582b9f84
出典データセット
uspto-grants-2014_09
特許番号
US08846955B2

反応ノート

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