Hydrochloric Acid → Focalin

HRID 599389

反応式

HRID 599389 の反応式
[CH3:1][O:2][C:3]([C@H:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C@@H:6]1[NH:11][CH2:10][CH2:9][CH2:8][CH2:7]1)=[O:4].[ClH:18]>C(O)(C)C.CO>[CH3:1][O:2][C:3]([C@@H:5]([C@@H:6]1[NH:11][CH2:10][CH2:9][CH2:8][CH2:7]1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)=[O:4].[ClH:18]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 154101Dexmethylphenidate

生成物 1

HCID 154100Focalin収率 86%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3776Isopropanol溶媒2 回

反応条件

温度
7.5 °C

実験手順

The organic layer was dewatered by azeotropic distillation under vacuum and was concentrated in vacuum to give D-threo-methylphenidate free base as an oil, which was used directly in hydrochloride salt formation. The solution of D-threo-methylphenidate free base in isopropanol (0.29 Kg) was charged to a jacketed vessel, cooled to 5-10° C. and treated with a solution of 37% HCl (78 g) in a mixture of isopropanol (40 g) and methanol (63 g) at less than 20° C. The formed slurry was cooled to 0 to 5° C., aged for 2 hours and filtered. The wet cake was washed with isopropanol (0.32 Kg total) in two portions and dried under vacuum at 45° C. for 16 hours to give Dexmethylphenidate hydrochloride (0.175 Kg, 0.649 mol, 86% yield) as a off-white solid; mp 206.4° C., ee 99.7%, α25D +83° (c 1 wt %, MeOH).

後処理

  1. temperatureThe formed slurry was cooled to 0 to 5° C.
  2. filtrationfiltered
  3. washThe wet cake was washed with isopropanol (0.32 Kg total) in two portions
  4. customdried under vacuum at 45° C. for 16 hours

出典と根拠

ORDレコード
ord-ed253010351a4d048e21b0b089654b1e
出典データセット
uspto-grants-2011_03
特許番号
US07897777B2

関連ノート

読み込み中…