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

Ammonium formate → 2-(cis-3-Methoxy-cyclohexyloxy)-pyridin-3-ylamine

HRID 406042
ノート
印刷プレビュー

反応式

HRID 406042 の反応式
C([O-])=O.[NH4+].[CH3:5][O:6][C@@H:7]1[CH2:12][CH2:11][CH2:10][C@H:9]([O:13][C:14]2[C:19]([N+:20]([O-])=O)=[CH:18][CH:17]=[CH:16][N:15]=2)[CH2:8]1>[Pd].CO.ClCCl.O>[CH3:5][O:6][C@@H:7]1[CH2:12][CH2:11][CH2:10][C@H:9]([O:13][C:14]2[C:19]([NH2:20])=[CH:18][CH:17]=[CH:16][N:15]=2)[CH2:8]1
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 2

HCID 2723923Ammonium formateHCID 673825062-(cis-3-Methoxy-cyclohexyloxy)-3-nitro-pyridine

生成物 1

HCID 673821972-(cis-3-Methoxy-cyclohexyloxy)-pyridin-3-ylamine

試薬・触媒・溶媒 4

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

Ammonium formate (7.25 g) was added to a suspension of 2-(cis-3-methoxy-cyclohexyloxy)-3-nitro-pyridine (5.80 g) and 10% palladium on charcoal (400 mg) in methanol (40 ml) at room temperature and the mixture was heated to reflux for 30 min until LCMS indicated complete conversion of the starting material. The mixture was diluted with dichloromethane (100 ml) and water (40 ml), filtered through celite, and the filtercake was washed with dichloromethane (30 ml). The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was submitted to column chromatography (silica gel, petrol ether/ethyl acetate 70:30) to give the desired product.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 30 min until LCMS
  3. filtrationfiltered through celite
  4. washthe filtercake was washed with dichloromethane (30 ml)
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-140377cf0a6d497e8153c8a12ccd715d
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08754079B2

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