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

Hydrogen Peroxide → HCID 13280944、化合物

HRID 1903629
ノート
印刷プレビュー

反応式

HRID 1903629 の反応式
OO.S(=O)(=O)(O)O.[Cl:8][C:9]1[CH:31]=[CH:30][C:12]2[C:13]3[C:14](=[CH:25][NH:26][C:27]=3[CH2:28][CH3:29])[CH2:15][N:16]=[C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:24])[C:11]=2[CH:10]=1.S(=O)(O)[O-:33].[Na+]>C(O)(=O)C>[Cl:8][C:9]1[CH:31]=[CH:30][C:12]2[C:13]3[CH:27]([CH2:28][CH3:29])[NH:26][C:25](=[O:33])[C:14]=3[CH2:15][N:16]=[C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:24])[C:11]=2[CH:10]=1
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 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 132809348-chloro-6-(2-chlorophenyl)-1-ethyl-2H,4H-pyrrolo[3,4-d][2]benzazepineHCID 23665763Sodium Bisulfite

生成物 1

HCID 13280944HCID 13280944、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

In one portion, 0.9 ml (7.9 mmol) of 30% hydrogen peroxide was added to 40 ml of a 1% solution of concentrated sulfuric acid in acetic acid. After stirring for 1 hour, 2.0 g (5.6 mmol) of 8-chloro-6-(2-chlorophenyl)-1-ethyl-2H,4H-pyrrolo[3,4-d][2]benzazepine were added, and the resulting mixture was stirred for 20 minutes. The excess peracid was discharged by the addition of saturated aqueous sodium bisulfite solution, and the mixture was concentrated at reduced pressure. The residue was partitioned between methylene chloride and water and neutralized with concentrated ammonium hydroxide solution. The methylene chloride solution was washed with brine, dried over anhydrous sodium sulfate, and concentrated at reduced pressure. The resulting oil was crystallized from ether to give 8-chloro-6-(2-chlorophenyl)-1-ethyl-1,4-dihydropyrrolo[3,4-d][2]benzazepin-3(2H)-one as yellow prisms, mp 233°-235° C. Recrystallization from a mixture of ethyl acetate and methanol gave colorless prims, mp 236°-237° C.

後処理

  1. stirringthe resulting mixture was stirred for 20 minutes
  2. concentrationthe mixture was concentrated at reduced pressure
  3. customThe residue was partitioned between methylene chloride and water and neutralized with concentrated ammonium hydroxide solution
  4. washThe methylene chloride solution was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated at reduced pressure
  7. customThe resulting oil was crystallized from ether

出典と根拠

ORDレコード
ord-a18503db013a497eb9fd3778341c3b5f
出典データセット
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04436662

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