Hydrochloric Acid → N-[(1R)-1-(4-{[(2S)-2-(4-fluorophenyl)morpholin-4-yl]methyl}phenyl)ethyl]methanesulfonamide hydrochloride

HRID 880243ノート

反応式

HRID 880243 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[O:13][CH2:12][CH2:11][N:10]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([C@H:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[CH3:22])=[CH:17][CH:16]=3)[CH2:9]2)=[CH:4][CH:3]=1.[ClH:28]>C(O)(C)C>[ClH:28].[F:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[O:13][CH2:12][CH2:11][N:10]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([C@H:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[CH3:22])=[CH:17][CH:16]=3)[CH2:9]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 71660507N-[(1R)-1-(4-{[(2S)-2-(4-Fluorophenyl)morpholin-4-yl]methyl}phenyl)ethyl]methanesulfonamide

生成物 1

HCID 71724619N-[(1R)-1-(4-{[(2S)-2-(4-fluorophenyl)morpholin-4-yl]methyl}phenyl)ethyl]methanesulfonamide hydrochloride収率 75%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

Dissolve N-[(1R)-1-(4-{[(2S)-2-(4-fluorophenyl)morpholin-4-yl]methyl}phenyl)ethyl]methanesulfonamide (50 g, 127.39 mmol) in isopropyl alcohol (200 mL). Add HCl (4M in dioxanes; 63.70 mL, 254.78 mmol) drop-wise to the solution and stir at ambient temperature for 50 min. Remove the volatiles under reduced pressure; add H2O (200 mL); then evaporate the water. Add H2O (200 mL) and isopropyl alcohol (100 mL), and concentrate to a total volume of 80 mL. Filter the resulting thick slurry; wash solid with H2O; collect by filtration; and dry the filter cake under reduced pressure at 55° C. to provide the title compound as a white solid (40.6 g, 75%). MS (m/z): 393 (M-Cl).

後処理

  1. customRemove the volatiles under reduced pressure
  2. customthen evaporate the water
  3. concentrationAdd H2O (200 mL) and isopropyl alcohol (100 mL), and concentrate to a total volume of 80 mL
  4. filtrationFilter the resulting thick slurry
  5. washwash solid with H2O
  6. filtrationcollect by filtration
  7. customand dry the filter cake under reduced pressure at 55° C.

出典と根拠

ORDレコード
ord-0bc9eda4bc894ec08a3a93dc362a7528
出典データセット
uspto-grants-2015_03
特許番号
US08993568B2

反応ノート

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