Hydrochloric Acid → Ticlopidine Hydrochloride

HRID 358817

반응식

HRID 358817 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 5472Ticlopidine

생성물 1

HCID 65335Ticlopidine Hydrochloride

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.)

후처리

  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

출처 및 근거

ORD 기록
ord-86835d43de4841bdb7b0d898875c2034
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997945

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