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 Bicarbonate → 3,4-Diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine

HRID 37492
ノート
印刷プレビュー

反応式

HRID 37492 の反応式
N[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]([N+:18]([O-:20])=[O:19])=[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[N:3]=1.B(F)(F)[F:28].F.N([O-])=O.[Na+].C(=O)([O-])O.[Na+]>C(O)(=O)C.O>[CH2:11]([O:10][C:8]([C:7]1[C:2]([F:28])=[N:3][C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:5]([N+:18]([O-:20])=[O:19])[C:6]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:9])[CH3:12]
参加物反応条件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 516892Sodium BicarbonateHCID 9855450Trifluoroborane HydrofluorideHCID 199356032-Amino-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridineHCID 23668193Sodium Nitrite

生成物 1

HCID 199356173,4-Diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 962Water溶媒

反応条件

温度
-5 °C

実験手順

In 2 ml of acetic acid was dissolved 100 mg of 2-amino-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, and 1.5 ml of 42% hydrofluoroboric acid was added to the solution. The mixture was cooled to -5° C., followed by adding dropwise a solution of 21 mg (1.1 eq) of sodium nitrite dissolved in 0.5 ml of water. Thirty minutes later, the temperature of the mixture was elevated to room temperature and the mixture was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. After the solvent was distilled off, the resulting crystals (2-pyridone compound) were collected by filtration with hexane, and washed. The solvent was distilled off from the obtained filtrate, to give an oily substance.

後処理

  1. additionwas added to the solution
  2. customThirty minutes
  3. customwas elevated to room temperature
  4. extractionfollowed by extraction with ethyl acetate
  5. washAfter the organic layer was washed with water
  6. dry with materiala saturated aqueous solution of sodium chloride, and dried
  7. distillationAfter the solvent was distilled off
  8. filtrationthe resulting crystals (2-pyridone compound) were collected by filtration with hexane
  9. washwashed
  10. distillationThe solvent was distilled off from the obtained filtrate
  11. customto give an oily substance

出典と根拠

ORDレコード
ord-4afe1d8998b646889314d45135528e41
出典データセット
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05420275

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート