Hexamethylenetetramine → 4-Hydroxy-3-methoxy-5-(trifluoromethyl)benzaldehyde

HRID 1088878ノート

反応式

HRID 1088878 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]([F:12])([F:11])[F:10])[C:4]=1[OH:13].C1N2CN3CN(C2)CN1C3.FC(F)(F)[C:26](O)=[O:27]>>[OH:13][C:4]1[C:5]([C:9]([F:11])([F:10])[F:12])=[CH:6][C:7]([CH:26]=[O:27])=[CH:8][C:3]=1[O:2][CH3:1]

参加物

4

反応物 3

HCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 151333362-Methoxy-6-(trifluoromethyl)phenol

生成物 1

HCID 193891994-Hydroxy-3-methoxy-5-(trifluoromethyl)benzaldehyde

実験手順

A solution containing 1.9 g of 2-methoxy-6-trifluoromethylphenol and 1.4 g of hexamethylenetetramine in 20 ml of trifluoroacetic acid was refluxed for 1 h. The solvent was removed in reduced pressure, 50 ml of 1 N hydrochloric acid was added to the residue and the solution was extracted with dichloromethane. Most part of the solvent was evaporated in vacuo and petroleum ether was added, whereupon the product crystallized. Yield 0.7 g (32%), m.p. 151°-152° C.

後処理

  1. temperaturewas refluxed for 1 h
  2. customThe solvent was removed in reduced pressure, 50 ml of 1 N hydrochloric acid
  3. additionwas added to the residue
  4. extractionthe solution was extracted with dichloromethane
  5. customMost part of the solvent was evaporated in vacuo and petroleum ether
  6. additionwas added, whereupon the product
  7. customcrystallized

出典と根拠

ORDレコード
ord-b9f9c015007847f4a55d8148e68249b2
出典データセット
uspto-grants-1990_10
特許番号
US04963590

反応ノート

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