Methylparaben → 4-(2-Piperidinoethoxy)benzoic acid hydrochloride

HRID 1290034노트

반응식

HRID 1290034 반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][CH:3]=1.Cl.[Cl:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+].C(OC(C)C)(=O)C>O>[ClH:13].[N:16]1([CH2:15][CH2:14][O:1][C:2]2[CH:11]=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=2)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1

참가 물질

6

반응물 4

HCID 7456MethylparabenHCID 7915Isopropyl AcetateHCID 11430Potassium CarbonateHCID 74826Piperidine, 1-(2-chloroethyl)-, hydrochloride

생성물 1

HCID 57438354-(2-Piperidinoethoxy)benzoic acid hydrochloride

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

To a 250 mL 3 neck flask equipped with mechanical stirring, condenser, and heating apparatus consisting of a RTD probe hooked via a temperature controller to a heating mantle and under nitrogen atmosphere, the following were added: 7.61 g methyl 4-hydroxybenzoate, 11.05 g β-chloroethylpiperidine hydrochloride, 16.59 g powdered potassium carbonate, and 60 ML isopropyl acetate. The mixture was heated slowly to 80° C. After 5 hours, high performance liquid chromatography showed reaction to be 90% complete. After being left overnight at 80° C., reaction was complete. The mixture was then cooled to ambient temperature, after which 60 mL deionized water was added. The mixture was stirred until all solids dissolved. The aqueous layer was separated and discarded.

후처리

  1. temperatureheating apparatus
  2. additionthe following were added
  3. customreaction
  4. waitAfter being left overnight at 80° C.
  5. customreaction
  6. temperatureThe mixture was then cooled to ambient temperature
  7. additionwas added
  8. dissolutiondissolved
  9. customThe aqueous layer was separated

출처 및 근거

ORD 기록
ord-e2319324dbf649da9e13f0233549441c
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750688

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