HRID1982309

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID280

Carbon dioxide

CO2

HCID962

Water

H2O

HCID6409

2,2,2-Trifluoroethanol

C2H3F3O

结构：CC[C@H](C)[C@H](NC(=O)OCc1ccccc1)C(=O)N[C@@H](Cc1c[nH]cn1)C(=O)N[C@@H](CCCCNC(=O)OC(C)(C)C)C(=O)OC

HCID178455965

未命名化合物

PRODUCTS

生成物

结构：CC[C@H](C)[C@H](N)C(=O)N[C@@H](Cc1c[nH]cn1)C(=O)N[C@@H](CCCCNC(=O)OC(C)(C)C)C(=O)OC

HCID178455961

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

8 g of Z-Ile-His-Lys(Boc)-OMe are suspended in a mixture of 80 ml of MeOH, 8 ml of H2O and 80 ml of trifluoroethanol, and hydrogenated with 800 mg of Pd-on-carbon (10% Pd) with CO2 -absorption until saturation, the initially undissolved material being dissolved. The catalyst is filtered off, the filtrate is concentrated to dryness and the resinous residue is crystallised from acetonitrile, yielding H-Ile-His-Lys(Boc)-OMe in the form of needles having a melting point of 129°-130°; Rf (I)=0.12; Rf (B)=0.14.

WORKUP

后处理

filtrationThe catalyst is filtered off
concentrationthe filtrate is concentrated to dryness
customthe resinous residue is crystallised from acetonitrile

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-95a49b717979440aadbf0bcee3f18bd7
来源数据集: uspto-grants-1986_06
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04595677
来源说明: uspto-grants-1986_06

反应 SMILES

[NH:1](C(OCC1C=CC=CC=1)=O)[C@H:2]([C:7]([NH:9][C@H:10]([C:17]([NH:19][C@H:20]([C:33]([O:35][CH3:36])=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][NH:25][C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])=[O:18])[CH2:11][C:12]1[N:16]=[CH:15][NH:14][CH:13]=1)=[O:8])[C@H:3]([CH2:5][CH3:6])[CH3:4].O.C(O)C(F)(F)F.C(=O)=O>CO>[NH2:1][C@H:2]([C:7]([NH:9][C@H:10]([C:17]([NH:19][C@H:20]([C:33]([O:35][CH3:36])=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][NH:25][C:26]([O:28][C:29]([CH3:30])([CH3:31])[CH3:32])=[O:27])=[O:18])[CH2:11][C:12]1[N:16]=[CH:15][NH:14][CH:13]=1)=[O:8])[C@H:3]([CH2:5][CH3:6])[CH3:4]