HCID 20186756, 화합물 → HCID 20186772, 화합물

HRID 2309010노트

반응식

HRID 2309010 반응식
[NH2:1][C:2]([CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH:13]([NH:15][CH2:16][CH:17]([C:22]2[CH:27]=[CH:26][C:25]([O:28]CC3C=CC=CC=3)=[CH:24][CH:23]=2)[O:18][CH2:19][CH2:20][OH:21])[CH3:14])=[CH:8][CH:7]=1)=[O:3].[H][H]>C(O)(=O)C.[Pd]>[NH2:1][C:2]([CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH:13]([NH:15][CH2:16][CH:17]([O:18][CH2:19][CH2:20][OH:21])[C:22]2[CH:23]=[CH:24][C:25]([OH:28])=[CH:26][CH:27]=2)[CH3:14])=[CH:8][CH:7]=1)=[O:3]

참가 물질

5

반응물 2

HCID 20186756HCID 20186756, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 20186772HCID 20186772, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

N-[2-(4-Aminocarbonylmethoxyphenyl)-1-methylethyl]-2-(4-benzyloxyphenyl)-2-(2-hydroxyethoxy)ethanamine (3.5 g) in glacial acetic acid (30 ml) was hydrogenated in the presence of 10% Palladium on carbon at atmospheric pressure and room temperature until hydrogen uptake was complete. The solution was filtered through diatomaceous earth and the solvent removed under vacuum. The residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate, the organic layer separated, dried (MgSO4) and evaporated to give an oil. The oil was crystallised from ethyl acetate to give the title compound, m.p. 145°-160° C. as a 40:60 mixture of diastereoisomers.

후처리

  1. filtrationThe solution was filtered through diatomaceous earth
  2. customthe solvent removed under vacuum
  3. customThe residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate
  4. customthe organic layer separated
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto give an oil
  8. customThe oil was crystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-a64b69f23e884ed786d7306f6684c519
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692465

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