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

HRID 1088878노트

반응식

HRID 1088878 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b9f9c015007847f4a55d8148e68249b2
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04963590

반응 노트

불러오는 중…