Sodium hydride → HCID 54229760, 화합물

HRID 1031503

반응식

HRID 1031503 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 54229760HCID 54229760, 화합물수율 31.7%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-b1d6e2d05cab486c9ad94dfadc2dbe51
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04954497

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