Acetic Acid → 4-Hydroxy-2,3,5-trimethylbenzaldehyde

HRID 85008

반응식

HRID 85008 반응식
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([CH3:9])[C:3]=1[OH:10].C1N2CN3CN(C2)CN1C3.[C:21](O)(=[O:23])C>>[CH3:8][C:7]1[C:2]([CH3:1])=[C:3]([OH:10])[C:4]([CH3:9])=[CH:5][C:6]=1[CH:21]=[O:23]

참가 물질

4

반응물 3

HCID 176Acetic AcidHCID 4101HexamethylenetetramineHCID 170162,3,6-Trimethylphenol

생성물 1

HCID 108990214-Hydroxy-2,3,5-trimethylbenzaldehyde

반응 조건

온도
115 °C

실험 절차

A mixture of 2,3,6-trimethylphenol (5 g, 0.036 mol) and hexamethylenetetramine (2.06 g, 0.0147 mol) in acetic acid (20 ml) was stirred at 115° C. for 2 hrs. The solvent (10 ml) was distilled and 20% (v/v) H2SO4 (20 ml) was added, and then the mixture was stirred at 115° C. for 20 min. The mixture was then poured on ice cold water (50 ml) and the separated solid was filtered, washed well with cold water (25 ml) and suck-dried. The wet cake was dried at 90° C. for 2 hrs under vacuum to yield 2,3,5-trimethyl-4-hydroxy-benzaldehyde (4.5 g, 75%; Table 1, no. 12).

후처리

  1. distillationThe solvent (10 ml) was distilled
  2. addition20% (v/v) H2SO4 (20 ml) was added
  3. stirringthe mixture was stirred at 115° C. for 20 min
  4. additionThe mixture was then poured on ice cold water (50 ml)
  5. filtrationthe separated solid was filtered
  6. washwashed well with cold water (25 ml)
  7. customsuck-dried
  8. customThe wet cake was dried at 90° C. for 2 hrs under vacuum

출처 및 근거

ORD 기록
ord-77f67864220348a6bc9a24e5108e2344
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846982B2

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