Hydrochloric Acid → Duloxetine Hydrochloride

HRID 1694626

反応式

HRID 1694626 の反応式
[CH3:1][NH:2][CH2:3][CH2:4][C@H:5]([O:11][C:12]1[CH:13]=[CH:14][CH:15]=[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=12)[C:6]1[S:10][CH:9]=[CH:8][CH:7]=1.[ClH:22]>CC(C)=O.C(OCC)C>[CH3:1][NH:2][CH2:3][CH2:4][C@H:5]([O:11][C:12]1[CH:13]=[CH:14][CH:15]=[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=12)[C:6]1[S:10][CH:9]=[CH:8][CH:7]=1.[ClH:22]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 60835Duloxetine

生成物 1

HCID 60834Duloxetine Hydrochloride収率 86%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 3283Diethyl Ether溶媒

実験手順

Duloxetine base (99% ee, 0.5 g, 1.68 mmoles) was dissolved in acetone (5 mL) and stirred with cooling in an ice-water bath. Hydrochloric acid in diethyl ether (2M, 0.8 mL) was added, and a precipitate formed within 2 minutes. The mixture was stirred at ambient temperature 16 hours, filtered and the collected solid washed with acetone (0.5 mL). The white solid was then dried under vacuum at ambient temperature to yield duloxetine hydrochloride (0.485 g, 1.45 mmoles, yield: 86%; Chiral HPLC: 99.5% ee).

後処理

  1. temperaturewith cooling in an ice-water bath
  2. customa precipitate formed within 2 minutes
  3. stirringThe mixture was stirred at ambient temperature 16 hours
  4. filtrationfiltered
  5. washthe collected solid washed with acetone (0.5 mL)
  6. customThe white solid was then dried under vacuum at ambient temperature

出典と根拠

ORDレコード
ord-503f92caa39a48a5874a234db96d37b6
出典データセット
uspto-grants-2012_04
特許番号
US08158808B2

関連ノート

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