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tert-Butanol → HCID 84013601、化合物

HRID 1481316
ノート
印刷プレビュー

反応式

HRID 1481316 の反応式
[O:1]1[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[C:3]([CH:10]=[O:11])=[CH:2]1.CC([OH:16])(C)C.CC(=CC)C.[O-]Cl=O.[Na+]>O>[O:1]1[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[C:3]([C:10]([OH:16])=[O:11])=[CH:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6386tert-ButanolHCID 105532-Methyl-2-buteneHCID 21794742Furo[2,3-b]pyridine-3-carbaldehydeHCID 23668197Sodium Chlorite

生成物 1

HCID 84013601HCID 84013601、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a suspension of furo[2,3-b]pyridine-3-carboxaldehyde (67 mmol) [J. Heterocyclic Chem., 23, 1465 (1986)] in 52 mL H2O were added NaH2PO4 (67 mmol), 260 mL t-BuOH, 71 mL 2-methyl-2-butene followed by portionwise addition of NaClO2 (100 mmol) at 0° C. After 15 min, the cooling bath was removed and the reaction was stirred at RT for 24 h. A solution of sat. aq. NaHCO3 was added and the mixture was extracted with EtOAc. The water phase was acidified with 1N HCl solution and it was then extracted 3 times with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo to obtain the desired compound as beige solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customthe cooling bath was removed
  2. additionA solution of sat. aq. NaHCO3 was added
  3. extractionthe mixture was extracted with EtOAc
  4. extractionwas then extracted 3 times with EtOAc
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-07584ecf2af24ffcb984e42830f28cf5
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09409917B2

反応ノート

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