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 → 6-[2-(2-Oxopiperazin-1-yl)ethyl]pyridine-3-carbonitrile

HRID 1466050
ノート
印刷プレビュー

反応式

HRID 1466050 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][NH:11][CH2:12][CH2:13][NH:14][C:15](=O)OC(C)(C)C)=[N:7][CH:8]=1)#[N:2].ClC[C:24](Cl)=[O:25].C(O)(C(F)(F)F)=O>C(Cl)Cl>[O:25]=[C:24]1[CH2:15][NH:14][CH2:13][CH2:12][N:11]1[CH2:10][CH2:9][C:6]1[N:7]=[CH:8][C:3]([C:1]#[N:2])=[CH:4][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 6577Chloroacetyl chlorideHCID 121005078tert-Butyl (2-{[2-(5-cyanopyridin-2-yl)ethyl]amino}ethyl)carbamate

生成物 1

HCID 895247896-[2-(2-Oxopiperazin-1-yl)ethyl]pyridine-3-carbonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

TEA (1 eq) was added dropwise to a solution of tert-Butyl (2-{[2-(5-cyanopyridin-2-yl)ethyl]amino}ethyl)carbamate (1 eq) and chloroacetyl chloride (1 eq) in 200 mL of DCM at 0° C. The mixture was stirred at room temperature for 30 minutes and washed with water and brine, dried over anhydrous Na2SO4 and condensed under vacuum. The resulting solid (1.0 g, 2.7 mmol) was added to the mixture of 10 mL TFA and 10 mL of DCM and stirred at RT for 1 hour then concentrated by vacuum. The residue was re-dissolved in CH3CN, K2CO3 was added and the mixture was stirred at RT for 2 hours. The mixture was poured into water and extracted with EtOAc twice. The combined organic layers were concentrated and the residue was purified by flash chromatography (DCM:MeOH=10:1) to afford the title compound 1H-NMR (400 MHz, CDCl3) δ ppm 8.74 (d, J=1.6 Hz, 1H), 7.81-7.83 (m, 1H), 7.31 (d, J=8.0 Hz, 1H), 3.71 (t, J=7.2 Hz, 2H), 3.42 (d, J=7.2 Hz, 2H), 3.24 (t, J=5.6 Hz, 2H), 3.09 (t, J=7.2 Hz, 2H), 2.98 (t, J=5.6 Hz, 2H).

後処理

  1. washwashed with water and brine
  2. dry with materialdried over anhydrous Na2SO4 and condensed under vacuum
  3. stirringstirred at RT for 1 hour
  4. concentrationthen concentrated by vacuum
  5. dissolutionThe residue was re-dissolved in CH3CN
  6. additionK2CO3 was added
  7. stirringthe mixture was stirred at RT for 2 hours
  8. additionThe mixture was poured into water
  9. extractionextracted with EtOAc twice
  10. concentrationThe combined organic layers were concentrated
  11. customthe residue was purified by flash chromatography (DCM:MeOH=10:1)

出典と根拠

ORDレコード
ord-26792eb4f3b44751b79f7e7510341d7b
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999990B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート