Sodium Hydroxide → 2-Chloro-1,10-phenanthroline

HRID 241395

反応式

HRID 241395 の反応式
S([O-])(O)(=O)=O.[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[C:19]([N:20]=1)=[C:18]1[C:13]([CH:14]=[CH:15][CH:16]=[N+:17]1[CH3:21])=[CH:12][CH:11]=2.[OH-:22].[Na+]>[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+]>[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[C:19](=[C:18]3[C:13](=[CH:12][CH:11]=2)[CH:14]=[CH:15][CH:16]=[N:17]3)[N:20]=1.[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[C:19]([N:20]=1)=[C:18]1[C:13]([CH:14]=[CH:15][C:16](=[O:22])[N:17]1[CH3:21])=[CH:12][CH:11]=2

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 866711149-Chloro-1-methyl-1,10-phenanthrolinium hydrogen sulfate

生成物 2

HCID 3551932-Chloro-1,10-phenanthrolineHCID 28475409-Chloro-1-methyl-1,10-phenanthrolin-2(1H)-one

試薬・触媒・溶媒 1

HCID 178511488HCID 178511488、化合物触媒

実験手順

To a stirred aqueous solution of potassium ferricyanide (22.1 g; 673 mmol) (200 mL) in an ice bath, compound (4) (6.17 g; 26.9 mmol) and an aqueous sodium hydroxide (16.14 g; 404 mmol) (110 mL) were alternately added over 20 minutes. The resulting reaction mixture was stirred in an ice bath, and further stirred at room temperature for 3.5 hours. Crude crystals which precipitated out were separated by filtration and dried, and then dissolved in methanol, and subsequently subjected to an activated carbon treatment. Then, a filtrate was concentrated under reduced pressure to give 4.26 g (yield: 72% from compound (3)) of the title compound (5).

後処理

  1. customThe resulting reaction mixture
  2. stirringfurther stirred at room temperature for 3.5 hours
  3. customCrude crystals which precipitated out
  4. customwere separated by filtration
  5. customdried
  6. dissolutiondissolved in methanol
  7. concentrationThen, a filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-094039dfcdf74fa7858037da8380279f
出典データセット
uspto-grants-2014_02
特許番号
US08648194B2

関連ノート

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