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

Sodium hydride → 3-bromo-N-(5-cyanopyridin-2-yl)-N-(oxetan-3-yl)pyrazolo[1,5-a]pyridine-5-carboxamide

HRID 539581
ノート
印刷プレビュー

反応式

HRID 539581 の反応式
[Br:1][C:2]1[CH:3]=[N:4][N:5]2[CH:10]=[CH:9][C:8]([C:11]([OH:13])=O)=[CH:7][C:6]=12.C(Cl)(=O)C(Cl)=O.[O:20]1[CH2:23][CH:22]([NH:24][C:25]2[CH:32]=[CH:31][C:28]([C:29]#[N:30])=[CH:27][N:26]=2)[CH2:21]1.[H-].[Na+]>ClCCl.CN(C)C=O>[Br:1][C:2]1[CH:3]=[N:4][N:5]2[CH:10]=[CH:9][C:8]([C:11]([N:24]([C:25]3[CH:32]=[CH:31][C:28]([C:29]#[N:30])=[CH:27][N:26]=3)[CH:22]3[CH2:21][O:20][CH2:23]3)=[O:13])=[CH:7][C:6]=12
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 24758Sodium hydrideHCID 65578Oxalyl chlorideHCID 457896763-Bromopyrazolo(1,5-a)pyridine-5-carboxylic acidHCID 867202576-(Oxetan-3-ylamino)nicotinonitrile

生成物 1

HCID 867202583-bromo-N-(5-cyanopyridin-2-yl)-N-(oxetan-3-yl)pyrazolo[1,5-a]pyridine-5-carboxamide収率 20%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒3 回

実験手順

To a solution of 3-bromopyrazolo[1,5-a]pyridine-5-carboxylic acid (I-7, 240 mg, 1 mmol) in dichloromethane (10 mL) was added oxalyl chloride (0.25 mL) and catalytic amounts of anhydrous dimethylformamide at rt. The reaction mixture was stirred for 30 minutes and subsequently the solvent was removed under reduced pressure. To the residual acid chloride was added a solution of 6-(oxetan-3-ylamino)nicotinonitrile (I-25, 175 mg, 1 mmol) in dichloromethane (10 mL). The resulting reaction mixture was quickly transferred to a microwave vial and NaH (60% in mineral oil) (191 mg, 5 mmol) was added. The vial was heatedin a microwave oven at 80° C. for 3 h. The reaction mixture was diluted with dichloromethane (15 mL) and subsequently washed with water, sat. NaHCO3 solution and brine. The organic layer was dried over Na2SO4 and the solvent was removed under reduced pressure. The resulting crude product was purified by column chromatography over silica gel (chloroform/MeOH, 0-10% EtOAc) to afford 75 mg (20%) of 3-bromo-N-(5-cyanopyridin-2-yl)-N-(oxetan-3-yl)pyrazolo[1,5-a]pyridine-5-carboxamide (I-26) as a brown solid. 1H NMR (400 MHz, CDCl3) δ 8.45 (d, J=7.0 Hz, 1H), 8.16 (s, 1H), 8.02 (t, J=7.90 Hz, 1H), 7.53 (d, J=0.8 Hz, 1H), 7.33-7.31 (m, 1H), 6.90-6.87 (m, 1H), 6.43 (d, J=10.1 Hz, 1H), 4.67-4.62 (m, 1H), 4.52-4.43 (m, 2H), 4.25-4.19 (m, 1H), 4.03-3.98 (m, 1H); ESI-LC/MS (m/z): [M+H]+ 398.13, [(M+2)+H]+ 400.08, RT 1.25 min.

後処理

  1. customsubsequently the solvent was removed under reduced pressure
  2. customThe resulting reaction mixture
  3. additionwas added
  4. waitThe vial was heatedin a microwave oven at 80° C. for 3 h
  5. washsubsequently washed with water, sat. NaHCO3 solution and brine
  6. dry with materialThe organic layer was dried over Na2SO4
  7. customthe solvent was removed under reduced pressure
  8. customThe resulting crude product was purified by column chromatography over silica gel (chloroform/MeOH, 0-10% EtOAc)

出典と根拠

ORDレコード
ord-07b83297c55443a4a82f7dd706acd8e5
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871754B2

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