Sodium Hydroxide → HCID 69859166、化合物

HRID 1456319ノート

反応式

HRID 1456319 の反応式
[N+:1]([C:4]1[C:5]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)=[N:6][CH:7]=[CH:8][CH:9]=1)([O-])=O.[H][H].[OH-].[Na+]>C(O)C.Cl>[C:13]1([CH3:16])[CH:12]=[CH:11][C:10]([C@H:5]2[C@@H:4]([NH2:1])[CH2:9][CH2:8][CH2:7][NH:6]2)=[CH:15][CH:14]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 11241348HCID 11241348、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 69859166HCID 69859166、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

A stirred solution of 3-nitro-2-p-tolylpyridine (5.0 g) in ethanol (200 ml) and concentrated hydrochloric acid (15 ml) was hydrogenated over pre-reduced platinum oxide (1.5 g) at 23°1 atm until hydrogen uptake was complete (~3 lh). The mixture was filtered through hyflo washing the pad of hyflo with water then the filtrate was evaporated in vacuo. Recrystallisation from isopropanol water gave a cream solid. The solid was treated with 2N sodium hydroxide solution and extracted with dichloromethane (5×200 ml). The combined organic extracts were dried (Na2SO4) and evaporated in vacuo to give the title compound as an orange-brown oil which partially crystallised on standing (2.20 g).

後処理

  1. filtrationThe mixture was filtered through hyflo
  2. washwashing the pad of hyflo with water
  3. customthe filtrate was evaporated in vacuo
  4. customRecrystallisation from isopropanol water
  5. customgave a cream solid
  6. extractionextracted with dichloromethane (5×200 ml)
  7. dry with materialThe combined organic extracts were dried (Na2SO4)
  8. customevaporated in vacuo

出典と根拠

ORDレコード
ord-2a46ad45f7984c92951b5851a3a48050
出典データセット
uspto-grants-1998_12
特許番号
US05843966

反応ノート

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