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

Ethyl Acetate → HCID 178485492、化合物

HRID 1633422
ノート
印刷プレビュー

反応式

HRID 1633422 の反応式
[CH3:1][N:2]=[C:3]([OH:19])[C:4]1[C:5](=[C:9]([N+]([O-])=O)[CH:10]=[C:11]([N+:13]([O-:15])=[O:14])[CH:12]=1)[C:6]([OH:8])=[O:7].C(OCC)(=O)C.C(=O)([O-])[O-].[K+].[K+].[Cl:32][C:33]1[CH:34]=[C:35]([SH:40])[CH:36]=[CH:37][C:38]=1[Cl:39]>O1CCCC1>[CH3:1][N:2]=[C:3]([OH:19])[C:4]1[C:5](=[C:9]([S:40][C:35]2[CH:36]=[CH:37][C:38]([Cl:39])=[C:33]([Cl:32])[CH:34]=2)[CH:10]=[C:11]([N+:13]([O-:15])=[O:14])[CH:12]=1)[C:6]([OH:8])=[O:7]
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 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 799643,4-DichlorobenzenethiolHCID 178485491HCID 178485491、化合物

生成物 1

HCID 178485492HCID 178485492、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

20.09 g (80 mmols) of 3,5-dinitrophthalic acid N-methylimide [prepared according to Example 2] are initially introduced into 300 ml of ethyl acetate and treated with 33.6 g (243 mmols) of ground, anhydrous potassium carbonate, and 15.04 g (84 mmols) of 3,4-dichlorothiophenol are then added dropwise at 25° C. After the addition of 100 ml of tetrahydrofuran, the mixture is stirred overnight and evaporated to dryness and the residue is taken up in a mixture of methylene chloride and dilute hydrochloric acid. The organic phase is washed with saturated NaCl solution, dried over sodium sulfate and evaporated. After recrystallisation from methylene chloride/n-pentane, 25.74 g (84% of theory) of the title imide, with a melting point of 167°-8° C., are obtained.

後処理

  1. additionare then added dropwise at 25° C
  2. customevaporated to dryness
  3. additionthe residue is taken up in a mixture of methylene chloride and dilute hydrochloric acid
  4. washThe organic phase is washed with saturated NaCl solution
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customAfter recrystallisation from methylene chloride/n-pentane, 25.74 g (84% of theory) of the title imide
  8. customwith a melting point of 167°-8° C., are obtained

出典と根拠

ORDレコード
ord-8a94a370355d4d39b82dadb2ca7a5edb
出典データセット
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04480105

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