Acetic Acid → 2,3,5,6-Pyridinetetramine

HRID 1172016

反応式

HRID 1172016 の反応式
O.Cl.Cl.Cl.[NH2:5][C:6]1[C:11]([NH2:12])=[CH:10][C:9]([NH2:13])=[C:8]([NH2:14])[N:7]=1.OC1C=C(C(O)=O)C(O)=CC=1C(O)=O.[Na+].[Na+].OC1C=C(C([O-])=O)C(O)=CC=1C([O-])=O.C(O)(=O)C>O.[OH-].[Na+]>[NH2:5][C:6]1[C:11]([NH2:12])=[CH:10][C:9]([NH2:13])=[C:8]([NH2:14])[N:7]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 691312,5-Dihydroxyterephthalic acidHCID 224757422,3,5,6-Tetraaminopyridine trihydrochloride monohydrate2 回HCID 178524618HCID 178524618、化合物

生成物 1

HCID 5868732,3,5,6-Pyridinetetramine

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 14798Sodium Hydroxide溶媒

実験手順

17.772 Parts by weight of 2,3,5,6-tetraaminopyridine trihydrochloride monohydrate was dissolved in 100 parts by weight of water deaerated with nitrogen. 13.208 Parts by weight of 2,5-dihydroxyterephthalic acid was dissolved in 137 parts by weight of a 1M sodium hydroxide aqueous solution, followed by deaeration with nitrogen. The 2,3,5,6-tetraaminopyridine trihydrochloride monohydrate aqueous solution was dropwise added to the 2,5-dihydroxyterephthalic acid disodium salt aqueous solution over 10 minutes. Then, 24.3 parts by weight of polyphosphoric acid, 35 parts by weight of water deaerated with nitrogen and 1 part by weight of acetic acid were added, and the resultant salt was recovered by filtering and dispersed in, and mixed with, 3,000 parts by weight of water deaerated with nitrogen, followed by re-filtering. Procedures of the above dispersing/mixing and filtering were repeated 3 times to give 2,3,5,6-tetraaminopyridine/2,5-dihydroxyterephthalaic acid salt.

後処理

  1. additionwere added
  2. customthe resultant salt was recovered
  3. filtrationby filtering
  4. additiondispersed in, and
  5. additionmixed with, 3,000 parts by weight of water
  6. filtrationby re-filtering
  7. additionProcedures of the above dispersing/mixing
  8. filtrationfiltering

出典と根拠

ORDレコード
ord-12a0db12f88e4371966cbe06ac3d9118
出典データセット
uspto-grants-2010_11
特許番号
US07833644B2

関連ノート

読み込み中…