Potassium Carbonate → 3-(2-Chloro-5-pyridylmethyl)-2-(nitroimino)thiazolidine

HRID 376994

反応式

HRID 376994 の反応式
[N+:1]([N:4]=[C:5]1[NH:9][CH2:8][CH2:7][S:6]1)([O-:3])=[O:2].C(=O)([O-])[O-].[K+].[K+].[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23]Cl)=[CH:19][N:18]=1>C(#N)C>[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][N:9]2[CH2:8][CH2:7][S:6][C:5]2=[N:4][N+:1]([O-:3])=[O:2])=[CH:19][N:18]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 1554792-Chloro-5-(chloromethyl)pyridineHCID 1362474392-Nitroiminothiazolidine

生成物 1

HCID 538802633-(2-Chloro-5-pyridylmethyl)-2-(nitroimino)thiazolidine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 2.9 g of 2-nitroiminothiazolidine, 2.9 g of anhydrous potassium carbonate, 3.2 g of 2-chloro-5-pyridylmethylchloride and 50 ml of acetonitrile was refluxed for 5 hours with vigorously stirring. After the reaction, most of the acetonitrile was removed by distillation and water was added to the residue. As the solid product was separated it was collected by filtration. The crude material was recrystallized from ethanol to give desired 3-(2-chloro-5-pyridylmethyl)-2-(nitroimino)thiazolidine.

後処理

  1. temperaturewas refluxed for 5 hours
  2. customAfter the reaction
  3. custommost of the acetonitrile was removed by distillation and water
  4. additionwas added to the residue
  5. customAs the solid product was separated it
  6. filtrationwas collected by filtration
  7. customThe crude material was recrystallized from ethanol

出典と根拠

ORDレコード
ord-8b3b96d21ac64d649fb6029ddf057354
出典データセット
uspto-grants-2000_02
特許番号
US06022967

関連ノート

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