Sodium hydride → HCID 54229760、化合物

HRID 1031503ノート

反応式

HRID 1031503 の反応式
[H-].[Na+].C(OP([CH2:11][C:12]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)=[O:13])(OCC)=O)C.[Cl:20][C:21]1[CH:45]=[CH:44][CH:43]=[CH:42][C:22]=1[O:23][C:24]1[CH:29]=[CH:28][C:27]([C:30](=O)[C:31]2[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[C:33]([O:39][CH3:40])[CH:32]=2)=[CH:26][N:25]=1>COCCOC>[Cl:20][C:21]1[CH:45]=[CH:44][CH:43]=[CH:42][C:22]=1[O:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]([C:31]2[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[C:33]([O:39][CH3:40])[CH:32]=2)=[CH:11][C:12]([N:14]2[CH2:15][CH2:16][O:17][CH2:18][CH2:19]2)=[O:13])=[CH:26][N:25]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 11207805Phosphonic acid, [2-(4-morpholinyl)-2-oxoethyl]-, diethyl esterHCID 14878846HCID 14878846、化合物

生成物 1

HCID 54229760HCID 54229760、化合物収率 31.7%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

In 1,2-dimethoxyethane (10 ml) was suspended 60% sodium hydride (dispersion in paraffin) (132 mg). To the suspension was added dropwise, while stirring, a solution of diethylphosphonoacetic acid morpholide (688 mg) in 1,2-dimethoxyethane (5 ml). To the mixture was added 2-(2-chlorophenoxy)-5-(3,4-dimethoxybenzoyl)pyridine (800 mg), which was heated for 8 hours under reflux. The reaction mixture was concentrated and the residue was dissolved in ether, washed with water and dried over anhydrous magnesium sulfate. The solvent was then distilled off to leave an oily substance, which was purified by means of a silica gel chromatography (eluted with ethyl acetate) to obtain 4-[3-(2-(2-chlorophenoxy)-5-pyridyl)-3-(3,4-dimethoxyphenyl)acryloyl]morpholine (Compound No.1) (330 mg) as a resinous solid.

後処理

  1. additionTo the suspension was added dropwise
  2. temperaturewas heated for 8 hours
  3. temperatureunder reflux
  4. concentrationThe reaction mixture was concentrated
  5. dissolutionthe residue was dissolved in ether
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was then distilled off
  9. customto leave an oily substance, which
  10. customwas purified by means of a silica gel chromatography (eluted with ethyl acetate)

出典と根拠

ORDレコード
ord-b1d6e2d05cab486c9ad94dfadc2dbe51
出典データセット
uspto-grants-1990_09
特許番号
US04954497

反応ノート

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