HRID1655308

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：CC[C@H](C)[C@H](NC(=O)CNC(=O)[C@@H](NC(=O)CNC(=O)OC(C)(C)C)C(C)C)C(=O)N1CCC[C@H]1C(=O)OCc1ccccc1

HCID131715771

未命名化合物

PRODUCTS

生成物

结构：CC[C@H](C)[C@H](NC(=O)CNC(=O)[C@@H](NC(=O)CNC(=O)OC(C)(C)C)C(C)C)C(=O)N1CCC[C@H]1C(=O)O

HCID131716314

未命名化合物

收率 97.6%

AUXILIARIES

试剂、催化剂与溶剂

催化剂HCID23938

Palladium

溶剂HCID176

Acetic Acid

C2H4O2

PROCEDURE

实验过程

III (7.8 g, 0.0123 mole) was taken in acetic acid (80 ml) and hydrogenated in the presence of 10% Pd-C (1 g) at 40 psi. After filtering the catalyst with the aid of celite, the solvent was removed under reduced pressure, triturated with ether, filtered, washed with ether then pet. ether and dried to obtain 6.5 g of the product (yield: 97.3%), m.p. shrinks at 127° C. and decomp. at 3 145° C. Rf3, 0.24; Rf4, 0.11. Anal. Calcd. for C25H43N5O10.1/2H2O: C 54.52, H 8.05, N 12.7%. Found: C 54.32, H 8.02, N 12.59%.

WORKUP

后处理

filtrationAfter filtering the catalyst with the aid of celite
customthe solvent was removed under reduced pressure
customtriturated with ether
filtrationfiltered
washwashed with ether
dry with materialpet. ether and dried

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-7877e6ab021746199a9bcb84f8b4e312
来源数据集: uspto-grants-1993_10
DOI: 10.6084/m9.figshare.5104873.v1
专利: US05250516
来源说明: uspto-grants-1993_10

反应 SMILES

[NH:1]([C:39]([O:41][C:42]([CH3:45])([CH3:44])[CH3:43])=[O:40])[CH2:2][C:3]([NH:5][C@H:6]([C:10]([NH:12][CH2:13][C:14]([NH:16][C@H:17]([C:22]([N:24]1[CH2:38][CH2:37][CH2:36][C@H:25]1[C:26]([O:28]CC1C=CC=CC=1)=[O:27])=[O:23])[C@H:18]([CH2:20][CH3:21])[CH3:19])=[O:15])=[O:11])[CH:7]([CH3:9])[CH3:8])=[O:4]>C(O)(=O)C.[Pd]>[NH:1]([C:39]([O:41][C:42]([CH3:45])([CH3:43])[CH3:44])=[O:40])[CH2:2][C:3]([NH:5][C@H:6]([C:10]([NH:12][CH2:13][C:14]([NH:16][C@H:17]([C:22]([N:24]1[CH2:38][CH2:37][CH2:36][C@H:25]1[C:26]([OH:28])=[O:27])=[O:23])[C@H:18]([CH2:20][CH3:21])[CH3:19])=[O:15])=[O:11])[CH:7]([CH3:9])[CH3:8])=[O:4]