Hydrochloric Acid → Ticlopidine Hydrochloride

HRID 358817

反応式

HRID 358817 の反応式
[ClH:1].C(O)(C)C.[CH:6]1[CH:7]=[CH:8][C:9]([Cl:22])=[C:10]([CH2:12][N:13]2[CH2:21][C:17]3[CH:18]=[CH:19][S:20][C:16]=3[CH2:15][CH2:14]2)[CH:11]=1>C1(C)C=CC=CC=1>[CH:6]1[CH:7]=[CH:8][C:9]([Cl:22])=[C:10]([CH2:12][N:13]2[CH2:21][C:17]3[CH:18]=[CH:19][S:20][C:16]=3[CH2:15][CH2:14]2)[CH:11]=1.[ClH:1]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 5472Ticlopidine

生成物 1

HCID 65335Ticlopidine Hydrochloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Gaseous HCl (0.22 g, 0.006 mole) is bubbled into 50 ml isopropanol. The resulting solution is added dropwise to ticlopidine free base (1.5 g, 0.005 mole) in 50 ml toluene, prepared, for example as described in Example A-3, maintaining the temperature below 40° C. during the addition. The reaction mixture is stirred for 1 hour, colled to about 5°-10° C. for 1 hour, and the precipitate separated by centrifugation. An acetone slurry is made of the precipitate, brought to reflux for 1 hour, and cooled to about 5°-10° C. for 1 hour. The precipitate, ticlopidine hydrochloride (Formula IV), is separated by centrifugation, dried at 65°-70° C. under vacuum, and recrystallized from methanol. (m.p. 206.5°-207.5° C.)

後処理

  1. temperaturemaintaining the temperature below 40° C.
  2. additionduring the addition
  3. waitcolled to about 5°-10° C. for 1 hour
  4. customthe precipitate separated by centrifugation
  5. temperatureto reflux for 1 hour
  6. temperaturecooled to about 5°-10° C. for 1 hour
  7. customThe precipitate, ticlopidine hydrochloride (Formula IV), is separated by centrifugation
  8. customdried at 65°-70° C. under vacuum
  9. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-86835d43de4841bdb7b0d898875c2034
出典データセット
uspto-grants-1991_03
特許番号
US04997945

関連ノート

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