Hexamethylenetetramine → HCID 21919188、化合物

HRID 1830213ノート

反応式

HRID 1830213 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 21919188HCID 21919188、化合物収率 27%

反応条件

温度
80 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-dd30e19c2c954e98a9878fb60b997825
出典データセット
uspto-grants-2006_06
特許番号
US07064124B2

反応ノート

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