Triethylamine → (S)-N-(1-(5-bromo-2-(methylamino)pyrimidin-4-yl)-2-(3,5-difluorophenyl)ethyl)-2-(3-(difluoromethyl)-4,4,7,7-tetrafluoro-4,5,6,7-tetrahydro-1H-indazol-1-yl)acetamide

HRID 2170333ノート

反応式

HRID 2170333 の反応式
[Br:1][C:2]1[C:3]([C@@H:12]([NH:22][C:23](=[O:41])[CH2:24][N:25]2[C:33]3[C:32]([F:35])([F:34])[CH2:31][CH2:30][C:29]([F:37])([F:36])[C:28]=3[C:27]([CH:38]([F:40])[F:39])=[N:26]2)[CH2:13][C:14]2[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([F:21])[CH:15]=2)=[N:4][C:5](S(C)(=O)=O)=[N:6][CH:7]=1.Cl.CN.[CH2:45]([N:47](CC)CC)C>ClCCl>[Br:1][C:2]1[C:3]([C@@H:12]([NH:22][C:23](=[O:41])[CH2:24][N:25]2[C:33]3[C:32]([F:35])([F:34])[CH2:31][CH2:30][C:29]([F:37])([F:36])[C:28]=3[C:27]([CH:38]([F:40])[F:39])=[N:26]2)[CH2:13][C:14]2[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([F:21])[CH:15]=2)=[N:4][C:5]([NH:47][CH3:45])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6364545Methylamine hydrochlorideHCID 90281385(S)-N-(1-(5-bromo-2-(methylsulfonyl)pyrimidin-4-yl)-2-(3,5-difluorophenyl)ethyl)-2-(3-(difluoromethyl)-4,4,7,7-tetrafluoro-4,5,6,7-tetrahydro-1H-indazol-1-yl)acetamide

生成物 1

HCID 90281536(S)-N-(1-(5-bromo-2-(methylamino)pyrimidin-4-yl)-2-(3,5-difluorophenyl)ethyl)-2-(3-(difluoromethyl)-4,4,7,7-tetrafluoro-4,5,6,7-tetrahydro-1H-indazol-1-yl)acetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To the mixture of compound 12C (68 mg, 0.1 mmol) and methylamine hydrochloride (34 mg, 0.5 mmol) in dichloromethane (5 ml) was added triethylamine (697 μL, 0.5 mmol). The reaction mixture was stirring at ambient temperature for 2 hours. The solvent was evaporated and the crude product was purified on reverse phase HPLC eluting with acetonitrile and water (with 0.1% TFA) to afford the title product. MS (m/z) 627.24 [M+H]+.

後処理

  1. customThe solvent was evaporated
  2. customthe crude product was purified on reverse phase HPLC
  3. washeluting with acetonitrile and water (with 0.1% TFA)

出典と根拠

ORDレコード
ord-23965a81b118492da7b073022a47815c
出典データセット
uspto-grants-2015_06
特許番号
US09050344B2

反応ノート

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