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

Sodium Hydroxide → ethyl 3-bromo-4-chloro-5-methyl-1H-pyrrole-2-carboxylate

HRID 1948381
ノート
印刷プレビュー

反応式

HRID 1948381 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[NH:5][C:6]=1[CH3:7].[Br:13]N1C(=O)CCC1=O.[OH-].[Na+]>ClCCl>[Br:13][C:3]1[C:2]([Cl:1])=[C:6]([CH3:7])[NH:5][C:4]=1[C:8]([O:10][CH2:11][CH3:12])=[O:9]
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 14798Sodium HydroxideHCID 67184N-bromobutanimideHCID 66707189ethyl 4-chloro-5-methyl-1H-pyrrole-2-carboxylate2 回

生成物 1

HCID 66707680ethyl 3-bromo-4-chloro-5-methyl-1H-pyrrole-2-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Ethyl 4-chloro-5-methyl-1H-pyrrole-2-carboxylate (Intermediate 7, 300 mg, 1.6 mmol) was dissolved in dry dichloromethane (10 ml), N-bromosuccinimide (285 mg, 1.6 mmol) was added at 0° C. and resulting mixture was stirred at room temperature over night. The mixture was poured into cold sodium hydroxide aqueous solution (2M) (20 ml), extracted with diethyl ether (2×20 ml). The organic phase was then washed with water (20 ml) and brine (20 ml), dried over anhydrous sodium sulfate, concentrated and purified by column chromatography (hexanes/ethyl acetate, gradient) to give the desired product as a yellowish solid. (424 mg).

後処理

  1. customresulting mixture
  2. extractionextracted with diethyl ether (2×20 ml)
  3. washThe organic phase was then washed with water (20 ml) and brine (20 ml)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. custompurified by column chromatography (hexanes/ethyl acetate, gradient)

出典と根拠

ORDレコード
ord-037a8d8369194bcc9d1c4f18c20ddb08
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399489B2

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