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

Lithium hydroxide, monohydrate → 6-[4-Methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylic acid

HRID 873519
ノート
印刷プレビュー

反応式

HRID 873519 の反応式
O.[OH-].[Li+].[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:17]=[C:16]([C:18]([O:20]C)=[O:19])[CH:15]=[CH:14][CH:13]=2)=[C:8]([CH3:22])[C:7]=1[CH:23]1[C:36]2[C:35](=[O:37])[CH2:34][C:33]([CH3:39])([CH3:38])[CH2:32][C:31]=2[O:30][C:29]2[CH2:28][C:27]([CH3:41])([CH3:40])[CH2:26][C:25](=[O:42])[C:24]1=2>O.C1COCC1>[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:17]=[C:16]([C:18]([OH:20])=[O:19])[CH:15]=[CH:14][CH:13]=2)=[C:8]([CH3:22])[C:7]=1[CH:23]1[C:24]2[C:25](=[O:42])[CH2:26][C:27]([CH3:40])([CH3:41])[CH2:28][C:29]=2[O:30][C:31]2[CH2:32][C:33]([CH3:39])([CH3:38])[CH2:34][C:35](=[O:37])[C:36]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 117700765Methyl 6-[4-methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylate

生成物 1

HCID 1177005176-[4-Methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylic acid収率 73.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒
2 回
HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of lithium hydroxide monohydrate (0.18 g, 4.36 mmol) in water (10.5 ml) was added dropwise to a solution of the methyl 6-[4-methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylate produced in Example 4-3 (1.05 g, 1.98 mmol) in THF (21 ml) at room temperature, and the mixture thus obtained was then stirred at the same temperature as above for 3 hours. Thereafter, water was added to the reaction solution, and the mixed solution was then washed with diethyl ether. Thereafter, a 1 N aqueous solution of hydrochloric acid (4.36 ml) was added to the water layer, and the mixed solution was then extracted with dichloromethane. The organic layer thus obtained was dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure, and the residue thus obtained was then washed with a mixed solution of diethyl ether and hexane, followed by collection by filtration and drying, to obtain the title compound (0.75 g, yield: 73%).

後処理

  1. customthe mixture thus obtained
  2. washthe mixed solution was then washed with diethyl ether
  3. additionThereafter, a 1 N aqueous solution of hydrochloric acid (4.36 ml) was added to the water layer
  4. extractionthe mixed solution was then extracted with dichloromethane
  5. customThe organic layer thus obtained
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled away under reduced pressure
  8. customthe residue thus obtained
  9. washwas then washed with a mixed solution of diethyl ether and hexane
  10. filtrationfollowed by collection by filtration
  11. customdrying

出典と根拠

ORDレコード
ord-181f711c211b4f17a4409227fb8fbb0d
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08975263B2

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