Methanesulfonic Acid → Rasagiline mesylate

HRID 401853ノート

反応式

HRID 401853 の反応式
[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

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 3052776Rasagiline

生成物 1

HCID 3052775Rasagiline mesylate収率 83.6%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

反応条件

温度
5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3ba668adc1934c91ba8d932d1597670e
出典データセット
uspto-grants-2014_06
特許番号
US08741962B2

反応ノート

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