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2-n-Butyl-5-hydroxymethyl-4-iodoimidazole → 2-Butyl-5-formyl-4-iodo-imidazole

HRID 2346
ノート
印刷プレビュー

反応式

HRID 2346 の反応式
[CH2:1]([C:5]1[NH:6][C:7]([CH2:11][OH:12])=[C:8]([I:10])[N:9]=1)[CH2:2][CH2:3][CH3:4]>ClCCl.[O-2].[O-2].[Mn+4]>[CH2:1]([C:5]1[NH:6][C:7]([CH:11]=[O:12])=[C:8]([I:10])[N:9]=1)[CH2:2][CH2:3][CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 148985472-n-Butyl-5-hydroxymethyl-4-iodoimidazole

生成物 1

HCID 1784182622-Butyl-5-formyl-4-iodo-imidazole収率 84.2%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

A stirred mixture of 174.1 g (0.62 mol) of 2-n-butyl-5-hydroxymethyl-4-iodoimidazole and 360 g (4.14 mol) of manganese dioxide in 3 L of dichloromethane was refluxed for 24 hr using a trap to remove water. The hot reaction mixture was filtered through a Celite® pad which was then washed with 4.5 L of boiling methylene chloride. The combined filtrates were concentrated to dryness. The residue was dissolved twice in 150 ml of methanol and each time the solution was concentrated to dryness. The residue was dissolved in 130 ml of methanol and chilled. After crystallization stopped, 700 ml of water was added slowly. The mixture was chilled, and the solid was collected by filtration, washed with water and dried to give 145.2 g (84%) of product; mp 104°-105° C.

後処理

  1. temperaturewas refluxed for 24 hr
  2. customto remove water
  3. filtrationThe hot reaction mixture was filtered through a Celite® pad which
  4. washwas then washed with 4.5 L of boiling methylene chloride
  5. concentrationThe combined filtrates were concentrated to dryness
  6. dissolutionThe residue was dissolved twice in 150 ml of methanol
  7. concentrationeach time the solution was concentrated to dryness
  8. dissolutionThe residue was dissolved in 130 ml of methanol
  9. temperaturechilled
  10. customAfter crystallization
  11. addition700 ml of water was added slowly
  12. temperatureThe mixture was chilled
  13. filtrationthe solid was collected by filtration
  14. washwashed with water
  15. customdried

出典と根拠

ORDレコード
ord-de21b1de13124c589802a272f7412025
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05728842

反応ノート

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