N-benzyloxycarbonyl-beta-benzyl-L-aspartyl-D-valine (R)-alpha-ethoxymethylbenzylamide → alpha-L-aspartyl-D-valine (R)-alpha-ethoxymethylbenzylamide

HRID 776

反应方程式

HRID 776 反应方程式
[CH2:1]([O:3][CH2:4][C@H:5]([NH:12][C:13](=[O:44])[C@@H:14]([CH:41]([CH3:43])[CH3:42])[NH:15][C:16](=[O:40])[C@H:17]([CH:29](CC1C=CC=CC=1)[C:30](=[O:32])[OH:31])[NH:18]C(OCC1C=CC=CC=1)=O)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH3:2]>CO.O.[Pd].[C]>[CH2:1]([O:3][CH2:4][C@H:5]([NH:12][C:13](=[O:44])[C@@H:14]([CH:41]([CH3:43])[CH3:42])[NH:15][C:16](=[O:40])[C@H:17]([CH2:29][C:30](=[O:31])[OH:32])[NH2:18])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH3:2]

参与物

5

反应物 1

HCID 54314208N-benzyloxycarbonyl-beta-benzyl-L-aspartyl-D-valine (R)-alpha-ethoxymethylbenzylamide

产物 1

HCID 54213385alpha-L-aspartyl-D-valine (R)-alpha-ethoxymethylbenzylamide收率 50.3%

试剂、催化剂与溶剂 3

HCID 178418390HCID 178418390，化合物催化剂HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

反应条件

温度
40 °C

实验过程

To a suspension of 1.20 g (1.99 mmols) of N-benzyloxycarbonyl-β-benzyl-L-aspartyl-D-valine (R)-α-ethoxymethylbenzylamide in 50 ml of methanol and 10 ml of water was added 0.30 g of 10% Pd-carbon (water content 50%). The mixture was reduced under hydrogen under heat at 40°C., 40 ml of water was added thereto, the catalyst was removed by filtration, and the resulting filtrate was concentrated under reduced pressure to 5 ml. The crystal thus precipitated was removed by filtration and dried to obtain 0.38 g (1.00 mmol, 50.3%) of α-L-aspartyl-D-valine (R)-α-ethoxymethylbenzylamide.

后处理

  1. customthe catalyst was removed by filtration
  2. concentrationthe resulting filtrate was concentrated under reduced pressure to 5 ml
  3. customThe crystal thus precipitated
  4. customwas removed by filtration
  5. customdried

来源与证据

ORD记录
ord-29bd294101a04d54b49813c6be393808
来源数据集
uspto-grants-1998_03
专利号
US05723165

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