Hydrochloric Acid → 3-Pyridinecarboxylic acid, (4-(3-(4-chlorophenyl)propoxy)phenyl)methyl ester

HRID 637475ノート

反応式

HRID 637475 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:17]=[CH:16][C:15]([CH2:18][OH:19])=[CH:14][CH:13]=2)=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl.[C:28](Cl)(=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[N:31][CH:30]=1>C1C=CC=CC=1.O>[C:28]([O:19][CH2:18][C:15]1[CH:14]=[CH:13][C:12]([O:11][CH2:10][CH2:9][CH2:8][C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)=[CH:17][CH:16]=1)(=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[N:31][CH:30]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 82604Nicotinoyl chlorideHCID 20256998HCID 20256998、化合物

生成物 1

HCID 30681633-Pyridinecarboxylic acid, (4-(3-(4-chlorophenyl)propoxy)phenyl)methyl ester

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962Water溶媒

実験手順

A mixture of 2.0 g (0.007 mole) of 4-[3-(4-chlorophenyl)propoxy)-phenylmethanol and 4.0 g triethylamine is added to 3.6 g (0.02 mole) of hydrochloride of nicotinoyl chloride in 50 ml of anhydrous benzene with stirring and the mixture is refluxed for 4 hrs. After cooling, water is added to the reaction mixture. The product is extracted with benzene and the extract is washed with water and dried over sodiun sulfate. Benzene is removed, the residual solid is recrystallized from ethanol to give a title compound in yield of 1.8 g (67.3%).

後処理

  1. temperaturethe mixture is refluxed for 4 hrs
  2. temperatureAfter cooling
  3. extractionThe product is extracted with benzene
  4. washthe extract is washed with water
  5. dry with materialdried over sodiun sulfate
  6. customBenzene is removed
  7. customthe residual solid is recrystallized from ethanol

出典と根拠

ORDレコード
ord-d330be54f5c34c50bd88d15c216931c0
出典データセット
uspto-grants-1985_12
特許番号
US04556715

反応ノート

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