Hydrochloric Acid → Levamisole

HRID 652557

反応式

HRID 652557 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]([CH:7]2[N:14]=[C:13]3[N:9]([CH2:10][CH2:11][S:12]3)[CH2:8]2)=[CH:5][CH:6]=1.Cl.Cl>O>[CH:1]1[CH:6]=[CH:5][C:4]([C@@H:7]2[N:14]=[C:13]3[N:9]([CH2:10][CH2:11][S:12]3)[CH2:8]2)=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 68628Tetramisole hydrochloride

生成物 1

HCID 26879Levamisole収率 124.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
45 °C

実験手順

A solution of 15.65 kg of levamisole.L-N-[(4-methoxyphenyl)sulfonyl]glutamic acid (salt) (30.02 mol) dissolved in 20.3 l water and 3,15 l sodium hydroxide 19.5 molar aqueous solution was extracted with 30.4 l of methylbenzene at 40° C. and the aqueous layer was washed with 7.5 l methylbenzene. Weighing of the combined water layers and determination of the concentration of the di-sodium salt of L-N-[(4-methoxyphenyl)sulfonyl]glutamic acid yields a 97% amount of di-sodium salt of L-N-[(4-methoxyphenyl)sulfonyl]glutamic acid. To the combined water layers were added 25.2 l water and 13.48 kg of tetramisole hydrochloride. After warming up at about 45° C. the aqueous solution was adjusted to pH 4.2 with hydrochloric acid and cooled at 15° C. After 18 hours the precipitate was filtered off, washed and dried under vacuo at 50° C. yielding 14.27 kg of levamisole.L-N-[(4-methoxyphenyl)sulfonyl]glutamic acid (salt) (yield: 97.7%); αD20 =- 64.1 (c5. 1N HCl); mp. 127.8°-129.3° C..

後処理

  1. temperaturecooled at 15° C
  2. filtrationAfter 18 hours the precipitate was filtered off
  3. washwashed
  4. customdried under vacuo at 50° C.

出典と根拠

ORDレコード
ord-15990f19218046059126ccabc67fb96d
出典データセット
uspto-grants-1987_06
特許番号
US04672126

関連ノート

読み込み中…