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

Dimethylformamide → Ethyl 7-((dimethylamino)thioxomethoxy)-4-oxo-8-propyl-4H-1-benzopyran-2-carboxylate

HRID 1034324
ノート
印刷プレビュー

反応式

HRID 1034324 の反応式
[OH:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=[O:15])[CH:7]=[C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[O:9][C:4]=2[C:3]=1[CH2:18][CH2:19][CH3:20].[H-].[Na+].CN(NC(Cl)=[S:28])C.[CH3:30][N:31]([CH3:34])[CH:32]=O>C(Cl)Cl>[CH3:34][N:31]([C:32](=[S:28])[O:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=[O:15])[CH:7]=[C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[O:9][C:4]=2[C:3]=1[CH2:18][CH2:19][CH3:20])[CH3:30]
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 6228DimethylformamideHCID 24758Sodium hydrideHCID 4196515Ethyl 7-hydroxy-4-oxo-8-propyl-4H-chromene-2-carboxylateHCID 14673822Dimethylaminothiocarbamylchloride

生成物 1

HCID 13744907Ethyl 7-((dimethylamino)thioxomethoxy)-4-oxo-8-propyl-4H-1-benzopyran-2-carboxylate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

Ethyl 7-hydroxy-4-oxo-8-n-propyl-4H-1-benzopyran-2-carboxylate (1 g) in anhydrous dimethylformamide (4 ml) is cooled to 0° and treated under nitrogen with sodium hydride (50% dispersion in mineral oil, 180 mg) with stirring for 30 minutes. Dimethylaminothiocarbamylchloride (465 mg) is added and the mixture is stirred 15 minutes at 0°, warmed to 80° and maintained as such for 18 hours. The mixture is cooled, diluted with methylene chloride (50 ml) and washed with water (3×100 ml)), dried over sodium sulfate and reduced to dryness in vacuo. The residue is recrystallized from ethyl acetate and hexane to yield the title compound.

後処理

  1. stirringthe mixture is stirred 15 minutes at 0°
  2. temperaturewarmed to 80°
  3. temperaturemaintained as such for 18 hours
  4. temperatureThe mixture is cooled
  5. washwashed with water (3×100 ml)),
  6. dry with materialdried over sodium sulfate
  7. customThe residue is recrystallized from ethyl acetate and hexane

出典と根拠

ORDレコード
ord-b34ba0936ec743b8aba301b1a89049fe
出典データセット
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05314918

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