Methanesulfonic Acid → Safinamide Mesylate

HRID 83473ノート

反応式

HRID 83473 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][CH:22]=1)[CH2:5][O:6][C:7]1[CH:19]=[CH:18][C:10]([CH2:11][NH:12][C@@H:13]([CH3:17])[C:14]([NH2:16])=[O:15])=[CH:9][CH:8]=1.[CH3:23][S:24]([OH:27])(=[O:26])=[O:25]>C(OCC)(=O)C>[CH3:23][S:24]([OH:27])(=[O:26])=[O:25].[F:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][CH:22]=1)[CH2:5][O:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:11][NH:12][C@@H:13]([CH3:17])[C:14]([NH2:16])=[O:15])=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 131682Safinamide

生成物 1

HCID 3038502Safinamide Mesylate収率 99.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
65 °C

実験手順

A mixture of (S)-2-[4-(3-fluorobenzyloxy)benzylamino]propanamide (20 g, 66 mmol, prepared in Example 12a) and ethyl acetate (510 g) is heated, under stirring up to 65° C. and kept under these conditions until a clear solution is obtained. Methanesulfonic acid (7 g, 72.6 mmol) is added in 40 min to the solution precooled to 55° C. The mixture is gradually cooled to 20° C. in 3 hours, kept at 20° C. for 2 hours. The heterogeneous mixture is filtered, the solid is dried at reduced pressure at 40° C. to yield 26.1 g of title compound as white powder (99% yield).

後処理

  1. temperatureis heated
  2. customis obtained
  3. customprecooled to 55° C
  4. temperatureThe mixture is gradually cooled to 20° C. in 3 hours
  5. filtrationThe heterogeneous mixture is filtered
  6. customthe solid is dried at reduced pressure at 40° C.

出典と根拠

ORDレコード
ord-0f665efc78a44a52ab336c047df35c59
出典データセット
uspto-grants-2014_09
特許番号
US08846763B2

反応ノート

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