1,4-Dioxane → HCID 46203865, 화합물

HRID 1724870노트

반응식

HRID 1724870 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 46203865HCID 46203865, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-61395ab9d01848f297c221b3f716704d
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07488740B2

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