Potassium Hydroxide → Cetirizine potassium

HRID 1248576

반응식

HRID 1248576 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][O:17][CH2:18][C:19]([O:21]C)=[O:20])[CH2:11][CH2:10]2)=[CH:4][CH:3]=1.[OH-].[K+:30]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[N:9]2[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][O:17][CH2:18][C:19]([O-:21])=[O:20])[CH2:13][CH2:14]2)=[CH:4][CH:3]=1.[K+:30]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 608480Cetirizine methyl ester

생성물 1

HCID 23711638Cetirizine potassium수율 56%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

16.8 g (0.0417 mole) of methyl 2-[2-[4-[(4-chlorophenyl)phenylmethyl]-1-piperazinyl]ethoxy]-acetate (prepared in the manner described above in Example 1.3) are dissolved in 65 ml of absolute ethanol. 42 ml of a 1 N ethanolic solution of potassium hydroxide are then added thereto and the reaction mixture is heated under reflux for 4 hours. It is then cooled and the precipitate removed by filitration, after washing with diethyl ether. The filtrate is evaporated to dryness and the evaporation residue is triturated with diethyl ether aand left to crystallize, 10.5 g of hydroscopic potassium 2-[2-[4-[(4-chlorophenyl)phenylmethyl]-1-piperazinyl]ethoxy]-acetate being obtained. The yield is 56% of theory; M.P. 161°-163° C.

후처리

  1. temperaturethe reaction mixture is heated
  2. temperatureunder reflux for 4 hours
  3. temperatureIt is then cooled
  4. customthe precipitate removed by filitration
  5. washafter washing with diethyl ether
  6. customThe filtrate is evaporated to dryness
  7. customthe evaporation residue is triturated with diethyl ether
  8. waitleft
  9. customto crystallize

출처 및 근거

ORD 기록
ord-28c43da10a344c36974a02b235cd667f
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04525358

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