Trifluoroacetic acid → N-(5-{4-[6-amino-5-(2,4-difluorobenzoyl)-2-oxopyridin-1(2H)-yl]-3,5-difluorophenoxy}pentyl)-L-leucine

HRID 1667387ノート

反応式

HRID 1667387 の反応式
[NH2:1][C:2]1[N:7]([C:8]2[C:32]([F:33])=[CH:31][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][NH:18][C@H:19]([C:24]([O:26]C(C)(C)C)=[O:25])[CH2:20][CH:21]([CH3:23])[CH3:22])=[CH:10][C:9]=2[F:34])[C:6](=[O:35])[CH:5]=[CH:4][C:3]=1[C:36](=[O:45])[C:37]1[CH:42]=[CH:41][C:40]([F:43])=[CH:39][C:38]=1[F:44].C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:1][C:2]1[N:7]([C:8]2[C:9]([F:34])=[CH:10][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][NH:18][C@H:19]([C:24]([OH:26])=[O:25])[CH2:20][CH:21]([CH3:23])[CH3:22])=[CH:31][C:32]=2[F:33])[C:6](=[O:35])[CH:5]=[CH:4][C:3]=1[C:36](=[O:45])[C:37]1[CH:42]=[CH:41][C:40]([F:43])=[CH:39][C:38]=1[F:44]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 57658405HCID 57658405、化合物

生成物 1

HCID 57658309N-(5-{4-[6-amino-5-(2,4-difluorobenzoyl)-2-oxopyridin-1(2H)-yl]-3,5-difluorophenoxy}pentyl)-L-leucine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

From Example 54. To a solution of tert-butyl N-(5-{4-[6-amino-5-(2,4-difluorobenzoyl)-2-oxopyridin-1(2H)-yl]-3,5-difluorophenoxy}pentyl)-L-leucinate (21 mg, 0.04 mmol) in DCM (2.5 ml) was added TFA (2.5 ml). The mixture was stirred at room temperature for 20 hours, before concentrating under reduced pressure. The residue was dissolved in minimal MeOH and azeotroped with 1:1 toluene/DCM three times. The title compound was afforded as a cream coloured solid as the mono-TFA salt (21 mg, 92% yield).

後処理

  1. concentrationbefore concentrating under reduced pressure
  2. dissolutionThe residue was dissolved in minimal MeOH
  3. customazeotroped with 1:1 toluene/DCM three times

出典と根拠

ORDレコード
ord-489157acda554c2db45f0124378e5239
出典データセット
uspto-grants-2011_10
特許番号
US08044211B2

反応ノート

読み込み中…