Sodium Carbonate → Methyl 4-(4-hydroxy-4-(2-hydroxyphenyl)piperidino)-2,2-diphenylbutyrate

HRID 279078

反応式

HRID 279078 の反応式
Br[CH2:2][CH2:3][C:4]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:5]([O:7][CH3:8])=[O:6].[OH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C:28]1([OH:34])[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1.C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[OH:34][C:28]1([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[OH:21])[CH2:29][CH2:30][N:31]([CH2:2][CH2:3][C:4]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:5]([O:7][CH3:8])=[O:6])[CH2:32][CH2:33]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 111062194-(2-Hydroxyphenyl)piperidin-4-olHCID 22624494Methyl 4-bromo-2,2-diphenylbutyrate

生成物 1

HCID 22624498Methyl 4-(4-hydroxy-4-(2-hydroxyphenyl)piperidino)-2,2-diphenylbutyrate収率 29.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

In 50 mL of anhydrous dimethylformamide were dissolved 2.24 g (6.7 mmol) of methyl 4-bromo-2,2-diphenylbutyrate and 1.30 g (6.7 mmol) of 4-(2-hydroxyphenyl)-4-piperidinol. To the resulting solution was added 1.07 g (10 mmol) of sodium carbonate, followed by stirring under heating at 50° C. for 35 hours. The residue obtained by distilling off the solvent under reduced pressure was dissolved in ethyl acetate, followed by washing with water and drying. The residue obtained by concentrating the solvent under reduced pressure was purified by chromatography on a silica gel column, whereby 870 mg (yield: 29.2%) of methyl 4-(4-hydroxy-4-(2-hydroxyphenyl)piperidino)-2,2-diphenylbutyrate was obtained.

後処理

  1. customThe residue obtained
  2. distillationby distilling off the solvent under reduced pressure
  3. dissolutionwas dissolved in ethyl acetate
  4. washby washing with water
  5. customdrying
  6. customThe residue obtained
  7. concentrationby concentrating the solvent under reduced pressure
  8. customwas purified by chromatography on a silica gel column

出典と根拠

ORDレコード
ord-59483b05e9344a2b9c35e2788b5cb54c
出典データセット
uspto-grants-2002_03
特許番号
US06362203B1

関連ノート

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