Hydrochloric Acid → Terbinafine Hydrochloride

HRID 1175204

反応式

HRID 1175204 の反応式
[CH3:1][C:2]([C:5]#[C:6]/[CH:7]=[CH:8]/[CH2:9][N:10]([CH2:12][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=12)[CH3:11])([CH3:4])[CH3:3].[ClH:23]>CC(C)=O>[CH3:4][C:2]([C:5]#[C:6]/[CH:7]=[CH:8]/[CH2:9][N:10]([CH2:12][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=12)[CH3:11])([CH3:1])[CH3:3].[ClH:23]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 1549008Terbinafine

生成物 1

HCID 5282481Terbinafine Hydrochloride収率 57.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
20 °C

実験手順

19.2 g crude terbinafine base (57.2 mmol theoretical, example 6) is dissolved in 83 ml acetone and then 6.2 ml (0.0631 mol) of 32% aqueous hydrochloric acid is added dropwise. The resulting suspension is stirred for 30 minutes at 20° C. and then cooled to −5°/−10° C. and stirred for a further 2.5 hours. The precipitate is filtered, washed with 16 ml cold acetone and dried to constant weight at 40° C. in a vacuum oven. 10.8 g (57.5% yield) terbinafine-HCl is obtained as a white solid with purity in excess of 99.8% (HPLC A %).

後処理

  1. temperaturecooled to −5°/−10° C.
  2. stirringstirred for a further 2.5 hours
  3. filtrationThe precipitate is filtered
  4. washwashed with 16 ml cold acetone
  5. customdried to constant weight at 40° C. in a vacuum oven

出典と根拠

ORDレコード
ord-9656c80af1014b1db5c11620bc6d11f4
出典データセット
uspto-grants-2010_11
特許番号
US07838704B2

関連ノート

読み込み中…