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 → 4-(2,3,4-Trimethoxy-6-methylbenzoyl)-2,3-dichloro-5-methoxypyridine

HRID 1835427
ノート
印刷プレビュー

反応式

HRID 1835427 の反応式
CN(C)C=O.P(Cl)(Cl)([Cl:8])=O.[CH3:11][O:12][C:13]1[C:30]([O:31][CH3:32])=[C:29]([O:33][CH3:34])[CH:28]=[C:27]([CH3:35])[C:14]=1[C:15]([C:17]1[C:22]([O:23][CH3:24])=[CH:21][N+:20]([O-])=[CH:19][C:18]=1[Cl:26])=[O:16]>C1(C)C=CC=CC=1>[CH3:11][O:12][C:13]1[C:30]([O:31][CH3:32])=[C:29]([O:33][CH3:34])[CH:28]=[C:27]([CH3:35])[C:14]=1[C:15]([C:17]1[C:22]([O:23][CH3:24])=[CH:21][N:20]=[C:19]([Cl:8])[C:18]=1[Cl:26])=[O:16]
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 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 235035884-(2,3,4-trimethoxy-6-methylbenzoyl)-3-chloro-5-methoxypyridine-N-oxide

生成物 1

HCID 235035954-(2,3,4-Trimethoxy-6-methylbenzoyl)-2,3-dichloro-5-methoxypyridine収率 739.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

5 ml of dimethylformamide was added to 2.5 ml of toluene, the mixture was cooled with ice, and 1.3 ml (1.4 mmol) of phosphorus oxychloride was dropwise added thereto. After the mixture was stirred under cooling with ice for 10 minutes, 2.5 g (0.7 mmol) of 4-(2,3,4-trimethoxy-6-methylbenzoyl)-3-chloro-5-methoxypyridine-N-oxide was added thereto. After the mixture was stirred under cooling with ice for 30 minutes, the temperature was recovered to room temperature, followed by stirring for 2 hours. 30 ml of water was added to the mixture to terminate the reaction, and ethyl acetate was added thereto for extraction. The organic layer was dried over anhydrous sodium sulfate, subjected to filtration and purified by silica gel column chromatography to obtain 2.0 g (yield 76%) of 4-(2,3,4-trimethoxy-6-methylbenzoyl)-2,3-dichloro-5-methoxypyridine (compound No. 193; m.p. 98-99° C.).

後処理

  1. additionwas dropwise added
  2. temperatureunder cooling with ice for 10 minutes
  3. stirringAfter the mixture was stirred
  4. temperatureunder cooling with ice for 30 minutes
  5. customthe temperature was recovered to room temperature
  6. stirringby stirring for 2 hours
  7. addition30 ml of water was added to the mixture
  8. customto terminate
  9. customthe reaction, and ethyl acetate
  10. additionwas added
  11. extractionfor extraction
  12. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  13. filtrationsubjected to filtration
  14. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-4e29c744629d4a6ba339a90cd7aeb21d
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06770662B2

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