1,4-Dioxane → HCID 46203865、化合物

HRID 1724870ノート

反応式

HRID 1724870 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([NH2:9])[CH:5]=[CH:4][N:3]=1.C([O-])(O)=O.[Na+].O1CCOCC1.Br.Br[CH2:23][C:24]([C:26]1[C:31]([C:32]([F:35])([F:34])[F:33])=[CH:30][CH:29]=[CH:28][N:27]=1)=O>O>[F:35][C:32]([F:33])([F:34])[C:31]1[C:26]([C:24]2[N:1]=[C:2]3[N:3]=[CH:4][CH:5]=[C:6]([NH2:9])[C:7]3=[N:8][CH:23]=2)=[N:27][CH:28]=[CH:29][CH:30]=1

参加物

6

反応物 4

HCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 22135565Pyridine-2,3,4-triamineHCID 462042022-Bromo-1-(3-trifluoromethyl-pyridin-2-yl)-ethanone hydrobromide

生成物 1

HCID 46203865HCID 46203865、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Dissolve 2,3,4-triaminopyridine (2.5 mmol) in water (20 mL). Add NaHCO3 (0.63 g, 7.5 mmol), dioxane (10 mL), and 2-bromo-1-(3-trifluoromethyl-pyridin-2-yl)-ethanone hydrobromide (0.5 g) and stir at 100° C. for 2 hours. Cool the mixture and extract with EtOAc (4×10 mL). Wash the combined organic extracts with brine and dry over Na2SO4. Purify the residue by preparative HPLC to give the title compound.

後処理

  1. temperatureCool the mixture
  2. extractionextract with EtOAc (4×10 mL)
  3. washWash the combined organic extracts with brine
  4. dry with materialdry over Na2SO4
  5. customPurify the residue by preparative HPLC

出典と根拠

ORDレコード
ord-61395ab9d01848f297c221b3f716704d
出典データセット
uspto-grants-2009_02
特許番号
US07488740B2

反応ノート

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