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

HRID 1667387노트

반응식

HRID 1667387 반응식
[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]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 57658405HCID 57658405, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-489157acda554c2db45f0124378e5239
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044211B2

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