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

HRID 637475노트

반응식

HRID 637475 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 82604Nicotinoyl chlorideHCID 20256998HCID 20256998, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 241Benzene용매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-d330be54f5c34c50bd88d15c216931c0
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556715

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