HCID 20186756、化合物 → HCID 20186772、化合物

HRID 2309010ノート

反応式

HRID 2309010 の反応式
[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]

参加物

5

反応物 2

HCID 20186756HCID 20186756、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 20186772HCID 20186772、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a64b69f23e884ed786d7306f6684c519
出典データセット
uspto-grants-1987_09
特許番号
US04692465

反応ノート

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