Hexamethylenetetramine → 3,5-Difluoro-4-hydroxybenzaldehyde

HRID 62833

反応式

HRID 62833 の反応式
[C:1](O)(C(F)(F)F)=[O:2].[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[C:10]=1[OH:16].C1N2CN3CN(C2)CN1C3>O>[F:8][C:9]1[CH:14]=[C:13]([CH:12]=[C:11]([F:15])[C:10]=1[OH:16])[CH:1]=[O:2]

参加物

5

反応物 3

HCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 943922,6-Difluorophenol

生成物 1

HCID 101925843,5-Difluoro-4-hydroxybenzaldehyde

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

TFA (7 mL) was added to 2,6-difluoro-phenol (1.0 g, 7.69 mmol) and hexam-ethylenetetraamine (1.08 g, 7.69 mmol), and the mixture was stirred at 75˜80° C. for 12 hours. The reactant was cooled, diluted with water, and then extracted with DCM/MeOH (9:1) solution three or four times. The organic layer was concentrated under reduced pressure, and DCM was added to the residue. The mixture was dried with MgSO4 and concentrated under reduced pressure. The reaction product was used in the next step without a separate purification process.

後処理

  1. temperatureThe reactant was cooled
  2. extractionextracted with DCM/MeOH (9:1) solution three or four times
  3. concentrationThe organic layer was concentrated under reduced pressure, and DCM
  4. additionwas added to the residue
  5. dry with materialThe mixture was dried with MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customThe reaction product was used in the next step without a separate purification process

出典と根拠

ORDレコード
ord-027e21b1ee4d42b3bf74111e4af661b8
出典データセット
uspto-grants-2016_09
特許番号
US09447044B2

関連ノート

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