Hydrochloric Acid → (S)-1-((R)-2,2,2-trifluoro-1-(3-(8-((R)-1-methoxypropan-2-yloxy)quinolin-2-yl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)ethyl)pyrrolidin-3-amine dihydrochloride

HRID 338958ノート

反応式

HRID 338958 の反応式
[F:1][C:2]([F:43])([F:42])[C@H:3]([N:29]1[CH2:33][CH2:32][C@H:31]([NH:34]C(=O)OC(C)(C)C)[CH2:30]1)[C:4]1[CH:5]=[CH:6][C:7]2[N:8]([C:10]([C:13]3[CH:22]=[CH:21][C:20]4[C:15](=[C:16]([O:23][C@H:24]([CH3:28])[CH2:25][O:26][CH3:27])[CH:17]=[CH:18][CH:19]=4)[N:14]=3)=[N:11][N:12]=2)[CH:9]=1.[ClH:44]>ClCCl>[ClH:44].[ClH:44].[F:42][C:2]([F:1])([F:43])[C@H:3]([N:29]1[CH2:33][CH2:32][C@H:31]([NH2:34])[CH2:30]1)[C:4]1[CH:5]=[CH:6][C:7]2[N:8]([C:10]([C:13]3[CH:22]=[CH:21][C:20]4[C:15](=[C:16]([O:23][C@H:24]([CH3:28])[CH2:25][O:26][CH3:27])[CH:17]=[CH:18][CH:19]=4)[N:14]=3)=[N:11][N:12]=2)[CH:9]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86707476tert-butyl (S)-1-((R)-2,2,2-trifluoro-1-(3-(8-((R)-1-methoxypropan-2-yloxy)quinolin-2-yl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)ethyl)pyrrolidin-3-ylcarbamate

生成物 1

HCID 86707477(S)-1-((R)-2,2,2-trifluoro-1-(3-(8-((R)-1-methoxypropan-2-yloxy)quinolin-2-yl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)ethyl)pyrrolidin-3-amine dihydrochloride収率 177.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl (S)-1-((R)-2,2,2-trifluoro-1-(3-(8-((R)-1-methoxypropan-2-yloxy)quinolin-2-yl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)ethyl)pyrrolidin-3-ylcarbamate (0.37 g, 0.61 mmol) in dichloromethane (1 mL) was added hydrochloric acid (5-6M in 2-propanol; 8.7 mL, 0.61 mmol). The reaction mixture was stirred at ambient temperature for 30 minutes. The solvent was removed under reduced pressure, and the resulting solid was suspended in acetonitrile (3 mL) and stirred at ambient temperature for 5 minutes. The solid was collected by vacuum filtration to give the title compound (0.31 g, 87%). LCMS APCI (+) m/z 501 (M+H). Specific rotation: [α]25D=0.48° (c=1.03, MeOH).

後処理

  1. customThe solvent was removed under reduced pressure
  2. stirringstirred at ambient temperature for 5 minutes
  3. filtrationThe solid was collected by vacuum filtration

出典と根拠

ORDレコード
ord-bd7855df3e4648c0b5265805ef9bcc5e
出典データセット
uspto-grants-2014_11
特許番号
US08889704B2

反応ノート

読み込み中…