Sodium Hydroxide → HCID 23359208、化合物

HRID 232870ノート

反応式

HRID 232870 の反応式
[OH-].[Na+].[C:3]([C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11]C)=[O:10])=[C:7]([CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)[CH:6]=1)#[N:4]>CO>[C:3]([C:5]1[CH:14]=[CH:13][C:8]([C:9]([OH:11])=[O:10])=[C:7]([CH2:15][O:16][C:17]2[CH:18]=[CH:19][C:20]([OH:23])=[CH:21][CH:22]=2)[CH:6]=1)#[N:4]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 23359186Methyl 4-cyano-2-[(4-hydroxyphenoxy)methyl]benzoate

生成物 1

HCID 23359208HCID 23359208、化合物収率 57.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

20 ml of a 3N-sodium hydroxide aqueous solution was added to 9.5 g of methyl 4-cyano-2-(4-hydroxyphenoxy)methylbenzoate obtained in Reference example 22 dissolved in 80 ml of methanol and the mixture was stirred at room temperature for 1.5 hours. After completion of the reaction, the solvent was removed under reduced pressure, water was added to the residue and the mixture was washed with diethyl ether and then adjusted to about pH 2 with conc. sulfuric acid. Crystals precipitated were collected by filtration and dissolved in ethyl acetate and the organic layer was washed with a saturated saline solution and then dried over anhydrous sodium sulfate. The solvent was removed from the solution to obtain 5.2 g of the title compound.

後処理

  1. customobtained in Reference example 22
  2. customAfter completion of the reaction
  3. customthe solvent was removed under reduced pressure, water
  4. additionwas added to the residue
  5. washthe mixture was washed with diethyl ether
  6. customCrystals precipitated
  7. filtrationwere collected by filtration
  8. dissolutiondissolved in ethyl acetate
  9. washthe organic layer was washed with a saturated saline solution
  10. dry with materialdried over anhydrous sodium sulfate
  11. customThe solvent was removed from the solution

出典と根拠

ORDレコード
ord-b51d0f5ed7534c8aadb14df8ff17d738
出典データセット
uspto-grants-1997_01
特許番号
US05591752

反応ノート

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