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

HRID 279078

반응식

HRID 279078 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-59483b05e9344a2b9c35e2788b5cb54c
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06362203B1

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