2-(2-hydroxy-ethyl-amino)-6-(4-benzyloxycarbonylamino-phenyl-amino)-9-ethyl-9H-purine → 6-(4-amino-phenyl-amino)-9-ethyl-2-(2-hydroxy-ethyl-amino)-9H-purine

HRID 9920

反応式

HRID 9920 の反応式
[OH:1][CH2:2][CH2:3][NH:4][C:5]1[N:13]=[C:12]2[C:8]([N:9]=[CH:10][N:11]2[CH2:14][CH3:15])=[C:7]([NH:16][C:17]2[CH:22]=[CH:21][C:20]([NH:23]C(OCC3C=CC=CC=3)=O)=[CH:19][CH:18]=2)[N:6]=1>CO.[Pd]>[NH2:23][C:20]1[CH:21]=[CH:22][C:17]([NH:16][C:7]2[N:6]=[C:5]([NH:4][CH2:3][CH2:2][OH:1])[N:13]=[C:12]3[C:8]=2[N:9]=[CH:10][N:11]3[CH2:14][CH3:15])=[CH:18][CH:19]=1

参加物

4

反応物 1

HCID 219882432-(2-hydroxy-ethyl-amino)-6-(4-benzyloxycarbonylamino-phenyl-amino)-9-ethyl-9H-purine

生成物 1

HCID 219882846-(4-amino-phenyl-amino)-9-ethyl-2-(2-hydroxy-ethyl-amino)-9H-purine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

0.45 g (1 mmol) of 2-(2-hydroxy-ethyl-amino)-6-(4-benzyloxycarbonylamino-phenyl-amino)-9-ethyl-9H-purine (prepared according to Example 107) are hydrogenated with 0.1 g of 10% Pd/C in 8 ml of methanol at RT for 5 h. The catalyst is filtered off, the residue on the filter is rinsed with dioxane/water (95:5) and the solvent is removed in vacuo. The desired compound, 6-(4-amino-phenyl-amino)-9-ethyl-2-(2-hydroxy-ethyl-amino)-9H-purine, can be isolated in crystalline form by this procedure; m.p. 210° C.; FAB-MS: (M+H)+=314; Rf=0.15 (methylene chloride:methanol=9:1).

後処理

  1. filtrationThe catalyst is filtered off
  2. washthe residue on the filter is rinsed with dioxane/water (95:5)
  3. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-070bedf9f90b4842b0782e22b1a25f04
出典データセット
uspto-grants-2006_08
特許番号
US07091346B1

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