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Hydrochloric Acid → HCID 10922198、化合物

HRID 1067595
ノート
印刷プレビュー

反応式

HRID 1067595 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([C:11]([CH3:16])([CH3:15])[C:12](O)=[O:13])[N:10]=2)[N:7]=1.[BH4-].C([N+](CCCC)(CCCC)CCCC)CCC.Cl>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([C:11]([CH3:16])([CH3:15])[CH2:12][OH:13])[N:10]=2)[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 169536Tetrabutylammonium borohydrideHCID 11746720HCID 11746720、化合物

生成物 1

HCID 10922198HCID 10922198、化合物収率 72.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

0.719 g of 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionic acid was dissolved in 15 ml of tetrahydrofuran; 0.535 g of N,N′-carbonyldiimidazole was added, followed by stirring at room temperature for 60 minutes. To this mixture, 1.15 g of tetra-n-butylammonium borohydride was added under ice cooling conditions, followed by stirring at room temperature for 1 hour. 2 ml of 5 N hydrochloric acid was added to the reaction mixture, followed by concentration under reduced pressure. The residue was ajusted to pH 7 by the addition of aqueous sodium carbonate and extracted with ethyl acetate; the extract was washed with saline and dried with magnesium sulfate. The dry product was concentrated under reduced pressure; the residue was subjected to silica gel column chromatography and eluted with ethyl acetate. The desired fraction was collected and concentrated; the crystal obtained was collected by filtration to yield 0.488 g of the title compound.

後処理

  1. stirringby stirring at room temperature for 1 hour
  2. concentrationfollowed by concentration under reduced pressure
  3. additionThe residue was ajusted to pH 7 by the addition of aqueous sodium carbonate
  4. extractionextracted with ethyl acetate
  5. washthe extract was washed with saline
  6. dry with materialdried with magnesium sulfate
  7. concentrationThe dry product was concentrated under reduced pressure
  8. washeluted with ethyl acetate
  9. customThe desired fraction was collected
  10. concentrationconcentrated
  11. customthe crystal obtained
  12. filtrationwas collected by filtration

出典と根拠

ORDレコード
ord-e367a675a2b145828d55dea0f332aad1
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06248740B1

反応ノート

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