Hexamethylenetetramine → HCID 21919188, 화합물

HRID 1245152노트

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HRID 1245152 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) followed by heating at 80° C. with stirring for 4 hours. After completion of the reaction, the solvent was evaporated therefrom, water (100 ml) was added to the resulting residue and the mixture was stirred for 30 minutes and extracted with methylene chloride. The extract was washed with water and dried, the solvent was evaporated therefrom and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to give the title compound (2.50 g, 7.23 mmol, 27%).

후처리

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated
  3. additionwater (100 ml) was added to the resulting residue
  4. stirringthe mixture was stirred for 30 minutes
  5. extractionextracted with methylene chloride
  6. washThe extract was washed with water
  7. customdried
  8. customthe solvent was evaporated
  9. customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-4ee18b72d32f40eea2ec1086efa3fcba
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122543B2

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