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

Hydrochloric Acid → 9-chloro-1,2-dihydro-4-hydroxy-1-methyl-2-oxo-3-phenyl-6H-pyrimido[2,1-a]isoindol-5-ium hydroxide

HRID 256697
ノート
印刷プレビュー

反応式

HRID 256697 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][NH:7][C:8]2=[N:11][CH3:12])=[CH:4][CH:3]=1.Cl.[OH-].[Na+].[C:16](=[C:18]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:19](Cl)=[O:20])=[O:17].N12CCCC1=NCCC2>C1(C)C=CC=CC=1.O>[OH-:17].[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][N+:7]3[C:16]([OH:17])=[C:18]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[C:19](=[O:20])[N:11]([CH3:12])[C:8]=32)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 763491,5-Diazabicyclo(4.3.0)non-5-eneHCID 107737343-Oxo-2-phenylprop-2-enoyl chlorideHCID 1356242226-Chloro-1-(methylimino)isoindoline

生成物 1

HCID 1784798909-chloro-1,2-dihydro-4-hydroxy-1-methyl-2-oxo-3-phenyl-6H-pyrimido[2,1-a]isoindol-5-ium hydroxide
収率 64.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒2 回

実験手順

A mixture of 5.42 g of 6-chloro-1-(methylimino)isoindoline (prepared from the hydrochloride by treatment with 1.5 equivalents of 2N sodium hydroxide solution) and 120 ml of toluene was treated dropwise under argon at 0-50 within 10 minutes with 5.96 g of α-carbonyl-phenylacetyl chloride. The mixture was stirred for 30 minutes, 4.47 g of 1,5-diazabicyclo[4.3.0]non-5-ene in 30 ml of toluene were subsequently added dropwise thereto, the mixture was stirred at 0-50 for a further 90 minutes, then treated with 50 ml of water and the separated crystals were filtered off under suction and washed with 35 ml of methylene chloride and, after drying, there was obtained 3.66 g of 9-chloro1,2-dihydro-4-hydroxy-1-methyl-2-oxo -3-phenyl-6H-pyrimido[2,1-a]isoindole-5-ium hydroxide (internal salt) with a m.p. of 245° (decomposition). This product was recrystallized from N,N-dimethylformamide and then had a m.p. of 288°.

後処理

  1. stirringthe mixture was stirred at 0-50 for a further 90 minutes
  2. filtrationthe separated crystals were filtered off under suction
  3. washwashed with 35 ml of methylene chloride
  4. customafter drying

出典と根拠

ORDレコード
ord-6668cfc4fe5f40478b199852ca427141
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05258387

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