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

Water → 1-(2-(4-((3,4-dihydro-2H-pyrano(2,3-c)pyridin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-methoxy-1,5-naphthyridin-2(1H)-one hydrochloride

HRID 1510792
ノート
印刷プレビュー

反応式

HRID 1510792 の反応式
[ClH:1].[O:2]1[C:7]2=[CH:8][N:9]=[C:10]([CH2:12][NH:13][CH:14]3[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][N:22]4[C:31]5[C:26](=[N:27][CH:28]=[C:29](F)[CH:30]=5)[CH:25]=[CH:24][C:23]4=[O:33])[CH2:16][CH2:15]3)[CH:11]=[C:6]2[CH2:5][CH2:4][CH2:3]1.C[O-].[Na+].CO.O.[C:40](OCC)(=[O:42])C>CO>[ClH:1].[O:2]1[C:7]2=[CH:8][N:9]=[C:10]([CH2:12][NH:13][CH:14]3[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][N:22]4[C:31]5[C:26](=[N:27][CH:28]=[C:29]([O:42][CH3:40])[CH:30]=5)[CH:25]=[CH:24][C:23]4=[O:33])[CH2:16][CH2:15]3)[CH:11]=[C:6]2[CH2:5][CH2:4][CH2:3]1
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 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 23694274Sodium methanolate methanolHCID 689273251-(2-(4-((3,4-dihydro-2H-pyrano(2,3-c)pyridin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-fluoro-1,5-naphthyridin-2(1H)-one hydrochloride

生成物 1

HCID 688927231-(2-(4-((3,4-dihydro-2H-pyrano(2,3-c)pyridin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-methoxy-1,5-naphthyridin-2(1H)-one hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of 60 mg of 1-(2-(4-((3,4-dihydro-2H-pyrano(2,3-c)pyridin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-fluoro-1,5-naphthyridin-2(1H)-one hydrochloride in 2 mL of methanol, 60 mg of a 28% sodium methoxide/methanol solution, and the mixture was heated under reflux while stirring for 4 hours. Thereto were added water and ethyl acetate, the organic layer was separated, and the aqueous layer was saturated with sodium chloride, and then extracted with ethyl acetate twice. The organic layer and the extract were combined, the resultant solution was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. To the resultant residue, 1 mL of ethyl acetate was added, and 1 mL of a 4.0 mol/L hydrogen chloride/ethyl acetate solution was added at room temperature. The solvent was distilled off under reduced pressure, ethyl acetate was added to the resultant residue, and the solid was filtered off to obtain 31 mg of 1-(2-(4-((3,4-dihydro-2H-pyrano(2,3-c)pyridin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-methoxy-1,5-naphthyridin-2(1H)-one hydrochloride as a yellow solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. customthe organic layer was separated
  4. extractionextracted with ethyl acetate twice
  5. dry with materialthe resultant solution was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionTo the resultant residue, 1 mL of ethyl acetate was added
  8. addition1 mL of a 4.0 mol/L hydrogen chloride/ethyl acetate solution was added at room temperature
  9. distillationThe solvent was distilled off under reduced pressure, ethyl acetate
  10. additionwas added to the resultant residue
  11. filtrationthe solid was filtered off

出典と根拠

ORDレコード
ord-4636eb8c44ea4bba87341db125200f37
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08211908B2

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