ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Trifluoroacetic acid → N-[3-[5-amino-6-(6-methyl-1H-benzimidazol-2-yl)pyrazin-2-yl]prop-2-ynyl]methanesulfonamide

HRID 1853141
ノート
印刷プレビュー

反応式

HRID 1853141 の反応式
[NH2:1][CH2:2][C:3]#[C:4][C:5]1[N:10]=[C:9]([C:11]2[N:15](C(OC(C)(C)C)=O)[C:14]3[CH:23]=[C:24]([CH3:27])[CH:25]=[CH:26][C:13]=3[N:12]=2)[C:8]([N:28](C(OC(C)(C)C)=O)C(OC(C)(C)C)=O)=[N:7][CH:6]=1.CCN(CC)CC.[S:50](Cl)([CH3:53])(=[O:52])=[O:51].C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:28][C:8]1[N:7]=[CH:6][C:5]([C:4]#[C:3][CH2:2][NH:1][S:50]([CH3:53])(=[O:52])=[O:51])=[N:10][C:9]=1[C:11]1[NH:15][C:14]2[CH:23]=[C:24]([CH3:27])[CH:25]=[CH:26][C:13]=2[N:12]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 86661949HCID 86661949、化合物

生成物 1

HCID 54597013N-[3-[5-amino-6-(6-methyl-1H-benzimidazol-2-yl)pyrazin-2-yl]prop-2-ynyl]methanesulfonamide収率 4%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

反応条件

温度
0 °C

実験手順

tert-Butyl 2-[6-(3-aminoprop-1-ynyl)-3-(bis(tert-butoxycarbonyl)amino)pyrazin-2-yl]-6-methyl-benzimidazole-1-carboxylate (90 mg, 0.1555 mmol) and Et3N (23.60 mg, 32.51 μL, 0.2332 mmol) were dissolved in DCM (10 mL) and cooled to 0° C. in and ice bath. Mesyl chloride (21.38 mg, 14.45 μL, 0.1866 mmol) as a solution in DCM (1 mL) was added dropwise and the reaction stirred at 0° C. for 20 minutes. The reaction mixture was washed with saturated aqueous NaHCO3 (×1) and brine (×1), dried (MgSO4), filtered and concentrated in vacuo. The residue was redissolved in DCM (10 mL) and TFA (177.3 mg, 119.8 μL, 1.555 mmol) added. The reaction mixture was stirred at ambient temperature for 1 hour then concentrated in vacuo. The residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 mM, 100 Å column, gradient 10%-95% B (solvent A: 0.05% TFA in water; solvent B: CH3CN) over 16 minutes at 25 mL/min]. The fractions were collected and freeze-dried to give the title compound as an yellow solid (2 mg, 4% Yield). 1H NMR (400.0 MHz, D4-MeOH) δ 1.6 (3H, s), 2.25 (3H, s), 3.25 (2H, s), 6.25 (1H, d), 6.55 (1H, s), 6.7 (1H, d), 7.3 (1H, s); MS (ES+) 357.

後処理

  1. washThe reaction mixture was washed with saturated aqueous NaHCO3 (×1) and brine (×1)
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. dissolutionThe residue was redissolved in DCM (10 mL)
  6. stirringThe reaction mixture was stirred at ambient temperature for 1 hour
  7. concentrationthen concentrated in vacuo
  8. customThe residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 mM, 100 Å column, gradient 10%-95% B (solvent A: 0.05% TFA in water; solvent B: CH3CN) over 16 minutes at 25 mL/min]
  9. customThe fractions were collected
  10. customfreeze-dried

出典と根拠

ORDレコード
ord-eca3677dd5a54da882ee380bd50fada5
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962631B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート