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

HRID 1290034

反応式

HRID 1290034 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 57438354-(2-Piperidinoethoxy)benzoic acid hydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e2319324dbf649da9e13f0233549441c
出典データセット
uspto-grants-1998_05
特許番号
US05750688

関連ノート

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