Hexamethylenetetramine → 3,5-Difluoro-4-hydroxybenzaldehyde
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
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
- temperatureThe reactant was cooled
- extractionextracted with DCM/MeOH (9:1) solution three or four times
- concentrationThe organic layer was concentrated under reduced pressure, and DCM
- additionwas added to the residue
- dry with materialThe mixture was dried with MgSO4
- concentrationconcentrated under reduced pressure
- 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
反応ノート
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