Sodium Hydroxide → (6-Ethoxy-benzofuran-3-yl)-methanol

HRID 1804790ノート

反応式

HRID 1804790 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].C([O:9][C:10]([C:12]1[C:16]2[CH:17]=[CH:18][C:19]([O:21][CH2:22][CH3:23])=[CH:20][C:15]=2[O:14][CH:13]=1)=O)C.[OH-].[Na+]>C1COCC1>[CH2:22]([O:21][C:19]1[CH:18]=[CH:17][C:16]2[C:12]([CH2:10][OH:9])=[CH:13][O:14][C:15]=2[CH:20]=1)[CH3:23]

参加物

5

反応条件

温度
0 °C

実験手順

1M LiAlH4-solution in THF (47.6 ml, 47.6 mmol) is diluted with 200 ml of THF and cooled to 0° C. 6-Ethoxy-benzofuran-3-carboxylic acid ethyl ester (27a) (5.6 g, 23.8 mmol) is dissolved in 100 ml of THF and added drop wise within 30 min. After completed addition the mixture is allowed to stir at 0° C. for 2 h. Then the reaction mixture is cooled to −15° C. and 10 ml of a 1M NaOH solution is added very slowly. Then the mixture is filtrated over celite, washed with THF and evaporated under reduced pressure.

後処理

  1. additionadded drop wise within 30 min
  2. additionaddition the mixture
  3. temperatureThen the reaction mixture is cooled to −15° C.
  4. filtrationThen the mixture is filtrated over celite
  5. washwashed with THF
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-04a5e50fb54a403ea26e168d592447c7
出典データセット
uspto-grants-2013_01
特許番号
US08354431B2

反応ノート

読み込み中…