Potassium Hydroxide → Cetirizine potassium

HRID 1248576

反応式

HRID 1248576 の反応式
[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]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 608480Cetirizine methyl ester

生成物 1

HCID 23711638Cetirizine potassium収率 56%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-28c43da10a344c36974a02b235cd667f
出典データセット
uspto-grants-1985_06
特許番号
US04525358

関連ノート

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