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 → HCID 89783772、化合物

HRID 1055862
ノート
印刷プレビュー

反応式

HRID 1055862 の反応式
[CH2:1]([NH:3][C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)[CH3:2].Cl[C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[C:14]([C:21]3[NH:29][C:28]4[CH2:27][CH2:26][NH:25][C:24](=[O:30])[C:23]=4[CH:22]=3)[CH:15]=[CH:16][CH:17]=2)[N:12]=1.C[Si]([N-][Si](C)(C)C)(C)C.[Na+].C(O)(C(F)(F)F)=O>C1COCC1.CS(C)=O>[CH2:1]([N:3]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)[C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[C:14]([C:21]3[NH:29][C:28]4[CH2:27][CH2:26][NH:25][C:24](=[O:30])[C:23]=4[CH:22]=3)[CH:15]=[CH:16][CH:17]=2)[N:12]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6422Trifluoroacetic acidHCID 2724254Sodium bis(trimethylsilyl)amide2 回HCID 11804744N-ethylpyridin-3-amineHCID 897835482-(2-chloroquinolin-8-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one

生成物 1

HCID 89783772HCID 89783772、化合物収率 11%

試薬・触媒・溶媒 2

HCID 679
Dimethyl Sulfoxide
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of N-ethylpyridin-3-amine (Enamine, Kiev, Ukraine; 0.164 g, 1.343 mmol) and 2-(2-chloroquinolin-8-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one (Example 1; 0.080 g, 0.269 mmol) was added NaHMDS (1.0 M in THF; 1.343 ml, 1.343 mmol). The dark red reaction was stirred for 30 min, then 0.5 mL 1.0 M NaHMDS in THF was added. After 30 min, the reaction was concentrated in vacuo and 2.5 mL DMSO and TFA (0.207 ml, 2.69 mmol) were added. Purified by rpHPLC (Phenomenex Gemini 150×30 mm C18 column, 5-60% ACN/H2O with 0.1% TFA); product-containing fractions were treated with saturated aq. NaHCO3 and DCM. The organic layer was separated, and the aq. layer was extracted 3×DCM. The combined organic layers were then dried over Na2SO4, filtered, and concentrated in vacuo to give 2-(2-(ethyl(pyridin-3-yl)amino)quinolin-8-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one (0.011 g, 0.029 mmol, 11% yield) as a solid: 1H NMR (400 MHz, DMSO-d6) δ ppm 11.97 (1H, br. s), 8.63-8.69 (1H, m), 8.55-8.62 (1H, m), 8.08 (1H, d, J=9.2 Hz), 7.99 (1H, dt, J=7.5, 0.7 Hz), 7.88 (1H, dt, J=8.2, 2.1 Hz), 7.53-7.63 (2H, m), 7.29 (1H, t, J=7.6 Hz), 6.99-7.07 (1H, m), 6.90-6.97 (2H, m), 4.11 (2H, q, J=7.0 Hz), 3.37-3.45 (2H, m), 2.66 (2H, t, J=6.9 Hz), 1.30 (3H, t, J=7.1 Hz). m/z (ESI, +ve) 384.2 (M+H)+.

後処理

  1. customThe dark red reaction
  2. waitAfter 30 min
  3. additionwere added
  4. customPurified by rpHPLC (Phenomenex Gemini 150×30 mm C18 column, 5-60% ACN/H2O with 0.1% TFA)
  5. additionproduct-containing fractions were treated with saturated aq. NaHCO3 and DCM
  6. customThe organic layer was separated
  7. extractionthe aq. layer was extracted 3×DCM
  8. dry with materialThe combined organic layers were then dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-88d2da4742ea43f992db3173f3a99c4a
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394297B2

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