Hexamethylenetetramine → HCID 21919188、化合物

HRID 1245152ノート

反応式

HRID 1245152 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) 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%).

後処理

  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)

出典と根拠

ORDレコード
ord-4ee18b72d32f40eea2ec1086efa3fcba
出典データセット
uspto-grants-2006_10
特許番号
US07122543B2

反応ノート

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