Hexamethylenetetramine → HCID 21919188, 화합물

HRID 1830213노트

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HRID 1830213 반응식
[CH3:1][O:2][C:3]1[C:4]([CH3:23])=[C:5]([C:14]([O:21][CH3:22])=[C:15]([O:19][CH3:20])[C:16]=1[O:17][CH3:18])[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13].C1N2CN3CN(C2)CN1C3.FC(F)(F)[C:36](O)=[O:37]>>[CH3:1][O:2][C:3]1[C:4]([CH3:23])=[C:5]([C:14]([O:21][CH3:22])=[C:15]([O:19][CH3:20])[C:16]=1[O:17][CH3:18])[CH2:6][C:7]1[C:8]([OH:13])=[C:9]([CH:10]=[CH:11][CH:12]=1)[CH:36]=[O:37]

참가 물질

4

반응물 3

HCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 219191522-(3,4,5,6-Tetramethoxy-2-methylbenzyl)phenol

생성물 1

HCID 21919188HCID 21919188, 화합물수율 27%

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온도
80 °C

실험 절차

2-(3,4,5,6-Tetramethoxy-2-methylbenzyl)phenol (8.64 g, 27.17 mmol) and hexamethylenetetramine (5.00 g, 35.67 mmol) were dissolved in trifluoroacetic acid (100 ml) and the solution was stirred under heating at 80° C. for 4 hours. After the completion of reaction, the solvent was removed by distillation and to the obtained residue, water (100 ml) was added. The resulting solution was stirred for 30 minutes and extracted with methylene chloride. The extract was washed with water and then dried, the solvent was removed by distillation and the obtained residue was purified by silica gel column chromatography (hexand:ethyl acetate=4:1) to obtain the titled compound (2.50 g, 7.23 mmol, 27%).

후처리

  1. customAfter the completion of reaction
  2. customthe solvent was removed by distillation and to the obtained residue, water (100 ml)
  3. additionwas added
  4. stirringThe resulting solution was stirred for 30 minutes
  5. extractionextracted with methylene chloride
  6. washThe extract was washed with water
  7. customdried
  8. customthe solvent was removed by distillation
  9. customthe obtained residue was purified by silica gel column chromatography (hexand:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-dd30e19c2c954e98a9878fb60b997825
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064124B2

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