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 Carbonate → HCID 57643118、化合物

HRID 2112930
ノート
印刷プレビュー

反応式

HRID 2112930 の反応式
Br[C:2]1[CH:7]=[CH:6][N:5]2[N:8]=[C:9]([NH:11][C:12]([NH:14][CH2:15][CH3:16])=[O:13])[N:10]=[C:4]2[CH:3]=1.[C:17]([O-:20])([O-])=O.[Na+].[Na+].CO[C:25]1[CH:26]=[N:27][CH:28]=[C:29](B(O)O)[CH:30]=1>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH2:15]([NH:14][C:12]([NH:11][C:9]1[N:10]=[C:4]2[CH:3]=[C:2]([C:25]3[CH:26]=[N:27][C:28]([O:20][CH3:17])=[CH:29][CH:30]=3)[CH:7]=[CH:6][N:5]2[N:8]=1)=[O:13])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 27630875-Methoxypyridine-3-boronic AcidHCID 57643071N-(7-Bromo[1,2,4]triazolo[1,5-a]pyridin-2-yl)-N′-ethylurea

生成物 1

HCID 57643118HCID 57643118、化合物

試薬・触媒・溶媒 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

Compound 4, prepared as in Example 1, (120 mg, 0.42 mmol) was dissolved in dioxane (5 mL), to which was added Na2CO3 (0.50 mL of a 2 M aqueous solution) and 3-methoxy-5-pyridineboronic acid (107 mg, 0.70 mmol). Pd(dppf)Cl2 (38 mg) was added last, and the mixture heated under nitrogen at reflux for 15 h. The reaction solvent was removed and the residue filtered through a plug of silica gel (gradient 2-5% MeOH/CH2Cl2 as eluant) to give a solid which was triturated with Et2O. 1-Ethyl-3-[7-(6-methoxy-pyridin-3-yl)-[1,2,4]triazolo[1,5-a]pyridin-2-yl]-urea was isolated mp. 230-233° C. Anal. calcd for C15H16N6O2: C, 57.7; H, 5.2; N, 26.9. Found: C, 57.6; H, 5.2; N, 26.4.

後処理

  1. temperaturethe mixture heated under nitrogen
  2. temperatureat reflux for 15 h
  3. customThe reaction solvent was removed
  4. filtrationthe residue filtered through a plug of silica gel (gradient 2-5% MeOH/CH2Cl2 as eluant)
  5. customto give a solid which
  6. customwas triturated with Et2O

出典と根拠

ORDレコード
ord-1c30c76f0615471381f6c06382bdeb0b
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07524860B2

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