Methanesulfonic Acid → Rasagiline mesylate

HRID 401853노트

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HRID 401853 반응식
[CH:1]#[C:2][CH2:3][NH:4][C@H:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6]1.[CH3:14][S:15]([OH:18])(=[O:17])=[O:16]>CC(O)C>[CH3:14][S:15]([OH:18])(=[O:17])=[O:16].[CH:1]#[C:2][CH2:3][NH:4][C@H:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6]1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 3052776Rasagiline

생성물 1

HCID 3052775Rasagiline mesylate수율 83.6%

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

반응 조건

온도
5 °C

실험 절차

Rasagiline base (81 g, 0.47 moles) was dissolved in IPA (810 ml) under stirring and the obtained solution was cooled to 5° C. A solution of methanesulfonic acid (0.49 moles, 47.7 g) in IPA (95 ml) was added dropwise to the above cooled solution. After complete addition, the mixture was stirred for 30 min at 5-10° C. to get the solid which was filtered and dried to get (105 g, 83%) of Rasagiline mesylate.

후처리

  1. additionAfter complete addition
  2. stirringthe mixture was stirred for 30 min at 5-10° C.
  3. customto get the solid which
  4. filtrationwas filtered
  5. customdried

출처 및 근거

ORD 기록
ord-3ba668adc1934c91ba8d932d1597670e
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741962B2

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