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

Pyridine → HCID 51030082、化合物

HRID 2036817
ノート
印刷プレビュー

反応式

HRID 2036817 の反応式
[C:1]1([C:7]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[C:9]([NH:27][CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=2)=[N:10][C:11]([C:17]2[CH:18]=[N:19][CH:20]=[C:21]([CH:26]=2)[C:22]([NH:24][NH2:25])=[O:23])=[N:12]3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:36](=O)[C:37]([O:39][CH3:40])=[O:38].C(=O)([O-])[O-].[K+].[K+].S(OS(C(F)(F)F)(=O)=O)(C(F)(F)F)(=O)=O.N1C=CC=CC=1>C(Cl)Cl.O>[C:1]1([C:7]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[C:9]([NH:27][CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=2)=[N:10][C:11]([C:17]2[CH:26]=[C:21]([C:22]4[O:23][C:36]([C:37]([O:39][CH3:40])=[O:38])=[N:25][N:24]=4)[CH:20]=[N:19][CH:18]=2)=[N:12]3)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 1049PyridineHCID 11430Potassium CarbonateHCID 67749Trifluoromethanesulfonic anhydrideHCID 79846Methyl chloroglyoxylateHCID 670559233-Pyridinecarboxylic acid, 5-[5-phenyl-4-[(2-pyridinylmethyl)amino]-2-quinazolinyl]-, hydrazide

生成物 1

HCID 51030082HCID 51030082、化合物
収率 79.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-(5-phenyl-4-(pyridin-2-ylmethylamino)quinazolin-2-yl)nicotinohydrazide (from Example 185, 0.30 g, 0.66 mmol) in DCM at 0° C. was added methyl 2-chloro-2-oxoacetate (0.062 mL, 0.66 mmol) and potassium carbonate (0.273 g, 1.90 mmol). Upon completion of addition, the mixture was stirred at RT for 16 h. After this time, water was added and the mixture was extracted into DCM, dried and concentrated. The resulting residue was dissolved in DCM. Triflic anhydride (0.187 mL, 1.1 mmol) and pyridine (0.149 mL, 1.8 mmol) were added and the resulting mixture was stirred at RT for 16 h. At the conclusion of this period, the reaction mixture was quenched with water and extracted with DCM (100 mL). The DCM layer was washed with water and brine. Chromatographic purification provided methyl 5-(5-(5-phenyl-4-(pyridin-2-ylmethylamino)quinazolin-2-yl)pyridin-3-yl)-1,3,4-oxadiazole-2-carboxylate (270 mg, 78% yield) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ (ppm): 9.81 (s, 1H), 9.17 (s, 1H), 9.09 (s, 1H), 8.24 (d, J=4.4 Hz, 1H), 7.94 (d, J=7.2 Hz, 1H), 7.86 (t, J=7.6 Hz, 1H), 7.75-7.72 (t, J=7.6 Hz, 3H), 7.59-7.51 (m, 5H), 7.34 (d, J=7.2 Hz, 2H), 7.24 (t, J=6.4 Hz, 1H), 6.98 (t, J=3.2 Hz, 1H), 4.77 (d, J=4.0 Hz, 2H). LCMS Method Q: retention time 1.39 min; [M+1]=514.5; HPLC Method B: purity 98.1%, retention time=8.74 min.

後処理

  1. additionUpon completion of addition
  2. extractionthe mixture was extracted into DCM
  3. customdried
  4. concentrationconcentrated
  5. dissolutionThe resulting residue was dissolved in DCM
  6. stirringthe resulting mixture was stirred at RT for 16 h
  7. customAt the conclusion of this period, the reaction mixture was quenched with water
  8. extractionextracted with DCM (100 mL)
  9. washThe DCM layer was washed with water and brine
  10. customChromatographic purification

出典と根拠

ORDレコード
ord-c37eaa1f9547493498a77055674cc1a5
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08575184B2

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