Trifluoroacetic acid → HCID 57691248、化合物

HRID 40289ノート

反応式

HRID 40289 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:9]=[CH:10][C:11]3[N:12]([C:14]([CH2:17][NH:18][C:19]4[C:28]5[C:23](=[CH:24][C:25]([O:29][CH3:30])=[CH:26][N:27]=5)[N:22]=[CH:21][CH:20]=4)=[N:15][N:16]=3)[N:13]=2)[CH:5]=[CH:4][C:3]=1[CH2:31][NH:32]C(=O)OC(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl.C(#N)C.O.[OH-].[Na+]>[NH2:32][CH2:31][C:3]1[CH:4]=[CH:5][C:6]([C:8]2[CH:9]=[CH:10][C:11]3[N:12]([C:14]([CH2:17][NH:18][C:19]4[C:28]5[C:23](=[CH:24][C:25]([O:29][CH3:30])=[CH:26][N:27]=5)[N:22]=[CH:21][CH:20]=4)=[N:15][N:16]=3)[N:13]=2)=[CH:7][C:2]=1[Cl:1]

参加物

6

反応物 2

HCID 6422Trifluoroacetic acidHCID 67967034Tert-butyl (2-chloro-4-(3-((7-methoxy-1,5-naphthyridin-4-ylamino)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)methylcarbamate

生成物 1

HCID 57691248HCID 57691248、化合物

試薬・触媒・溶媒 3

HCID 14798Sodium Hydroxide触媒HCID 6344Dichloromethane溶媒HCID 18373917Acetonitrile--water (1/1)溶媒

反応条件

温度
23 °C

実験手順

To a stirring solution of tert-butyl (2-chloro-4-(3-((7-methoxy-1,5-naphthyridin-4-ylamino)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)methylcarbamate (70 mg, 128 μmol) in DCM (2 mL) was added TFA (2 mL). Reaction solution stirred for 30 min at 23° C. Solvents then removed under reduced pressure and residue purified on prep-HPLC using a water/ACN (0.1% TFA) gradient. Resulting solid was dissolved in 1:1 ACN/water (1 mL) and pH adjusted to 10 with 1M NaOH (approx 10 drops). Resulting solid collected by filtraton and washed with water (5 mL). MS (ESI pos. ion) m/z: 447 (MH+). Calc'd exact mass for C22H19ClN8O: 446.

後処理

  1. customReaction solution
  2. customSolvents then removed under reduced pressure and residue
  3. custompurified
  4. customResulting solid
  5. customResulting solid
  6. customcollected by filtraton
  7. washwashed with water (5 mL)

出典と根拠

ORDレコード
ord-d4dc1748ec254723980e1d3042b23aa1
出典データセット
uspto-grants-2013_09
特許番号
US08524900B2

反応ノート

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