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

Potassium Carbonate → HCID 10158642、化合物

HRID 899390
ノート
印刷プレビュー

反応式

HRID 899390 の反応式
[N:1]1[O:2][N:3]=[C:4]2[CH:9]=[C:8]([O:10][C:11]3[N:30]=[CH:29][CH:28]=[CH:27][C:12]=3[C:13]([NH:15][CH2:16][C:17]3[CH:22]=[CH:21][C:20]([C:23](O)([CH3:25])[CH3:24])=[CH:19][CH:18]=3)=[O:14])[CH:7]=[CH:6][C:5]=12.C[Si]([C:35]#[N:36])(C)C.[Sn](Cl)(Cl)(Cl)Cl.C(=O)([O-])[O-].[K+].[K+].O.O.[F-].[K+]>ClCCl.O>[N:1]1[O:2][N:3]=[C:4]2[CH:9]=[C:8]([O:10][C:11]3[N:30]=[CH:29][CH:28]=[CH:27][C:12]=3[C:13]([NH:15][CH2:16][C:17]3[CH:18]=[CH:19][C:20]([C:23]([C:35]#[N:36])([CH3:25])[CH3:24])=[CH:21][CH:22]=3)=[O:14])[CH:7]=[CH:6][C:5]=12
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 11430Potassium CarbonateHCID 24287Tin tetrachlorideHCID 82115Trimethylsilyl cyanideHCID 98659292-(2,1,3-Benzoxadiazol-5-yloxy)-N-((4-(1-hydroxy-1-methylethyl)phenyl)methyl)-3-pyridinecarboxamideHCID 23708904Potassium fluoride dihydrate

生成物 1

HCID 10158642HCID 10158642、化合物
収率 40.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-(benzo[2,1,3]oxadiazol-5-yloxy)-N-[4-(1-hydroxy-1-methyl-ethyl)-benzyl]-nicotinamide (300 mg, 0.74 mmol) in dichloromethane (1.5 ml) cooled to 0° C. was added trimethylsilyl cyanide (1 ml, 7.4 mmol) followed by slow addition of tin tetrachloride (7 drops of a 1.0 M solution in dichloromethane). The reaction mixture was allowed to warm to room temperature overnight. Potassium carbonate (300 mg, 2.10 mmol) and potassium fluoride dihydrate (120 mg, 2.10 mmol) were added, followed by dropwise addition of water. The reaction mixture was stirred vigorously for 90 m., after which silica gel was (600 mg) added. The mixture was filtered and washed thoroughly with dichloromethane. The filtrate was washed with saturated aqueous sodium bicarbonate, dried over magnesium sulfate, filtered and concentrated to give 124 mg of a pale yellow solid. Product was recrystallized from ethyl acetate/hexane to afford 96 mg (31% yield) of a pale yellow solid.

後処理

  1. additionadded
  2. filtrationThe mixture was filtered
  3. washwashed thoroughly with dichloromethane
  4. washThe filtrate was washed with saturated aqueous sodium bicarbonate
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-a64eaedaea9147e98dd4d01ceb404108
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07354941B2

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