Water → Benzene, 1-((2-(4-(ethoxymethoxy)phenyl)-2-methylpropoxy)methyl)-3-phenoxy-

HRID 434534ノート

反応式

HRID 434534 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([CH3:28])([CH3:27])[CH2:11][O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:15]=2)=[CH:6][CH:5]=1.Cl[CH2:30][O:31][CH2:32][CH3:33].O>O1CCCC1>[CH2:32]([O:31][CH2:30][O:3][C:4]1[CH:5]=[CH:6][C:7]([C:10]([CH3:28])([CH3:27])[CH2:11][O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:15]=2)=[CH:8][CH:9]=1)[CH3:33]

参加物

6

反応物 4

HCID 962WaterHCID 18523Chloromethyl ethyl etherHCID 24758Sodium hydrideHCID 157700Phenol, 4-(1,1-dimethyl-2-((3-phenoxyphenyl)methoxy)ethyl)-

生成物 1

HCID 3067186Benzene, 1-((2-(4-(ethoxymethoxy)phenyl)-2-methylpropoxy)methyl)-3-phenoxy-

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 50 ml dry tetrahydrofuran was added 1.0 g of sodium hydride (60% in oil) and then 5.0 g of 3-phenoxybenzyl 2-(4-hydroxyphenyl)-2-methylpropyl ether in 15 ml of dry tetrahydrofuran was added dropwise to the mixture under reflux over a period of 30 minutes. The mixture was further refluxed for 10 minutes and 5.0 ml of ethyl chloromethyl ether was added dropwise to the mixture for 30 minutes. And the resulting mixture was further refluxed for 10 minutes, cooled to room temperature, poured into water, and extracted with benzene. The benzene extract was washed with water, dried over Na2SO4, and evaporated to give the oily residue which was purified by column chromatography on 150 g silica gel (20:1 mixed solvent of benzene and ether was used as eluent) to give 5.0 g of 3-phenoxybenzyl 2-(4-ethoxymethoxyphenyl)-2-methylpropyl ether.

後処理

  1. temperatureunder reflux over a period of 30 minutes
  2. temperatureThe mixture was further refluxed for 10 minutes
  3. temperatureAnd the resulting mixture was further refluxed for 10 minutes
  4. extractionextracted with benzene
  5. extractionThe benzene extract
  6. washwas washed with water
  7. dry with materialdried over Na2SO4
  8. customevaporated
  9. customto give the oily residue which
  10. customwas purified by column chromatography on 150 g silica gel (20:1 mixed solvent of benzene and ether was used as eluent)

出典と根拠

ORDレコード
ord-9b2029a77fda48428a25d4f01a8b4dfa
出典データセット
uspto-grants-1983_08
特許番号
US04397864

反応ノート

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