HRID65353

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：CC(C)(C)OC(=O)CCCCCCC[NH-].CC(C)C[C@H](NC(=O)[C@H](Cc1c[nH]cn1)NC(=O)[C@H](Cc1ccccc1)NC(=O)OCc1ccccc1)C(=O)N[C@H](C(=O)O)C(C)C

HCID178450968

未命名化合物

PRODUCTS

生成物

结构：CC(C)C[C@H](NC(=O)[C@H](Cc1c[nH]cn1)NC(=O)[C@H](Cc1ccccc1)NC(=O)OCc1ccccc1)C(=O)N[C@H](C(=O)O)C(C)C.[NH-]CCCCCCCC(=O)O

HCID178445988

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6422

未命名化合物

PROCEDURE

实验过程

63 mg of Z-Phe-His-Leu-Val-7-tert.-butoxycarbonylheptyl amide (Example 28) are stirred for 10 minutes at room temperature in 1.5 ml of trifluoroacetic acid. The resulting solution is concentrated. The residue is purified by flash chromatography (30 g of silica gel 60, 40-63 μm, approximately 0.4 bar, eluant B1). The productcontaining fractions are combined and concentrated by evaporation. The residue is stirred in 2 ml of water, the solid portion is filtered off with suction and dried in a high vacuμmand the title compound is obtained in the form of a white powder. Rf (B11)=0.14.

WORKUP

后处理

concentrationThe resulting solution is concentrated
customThe residue is purified by flash chromatography (30 g of silica gel 60, 40-63 μm, approximately 0.4 bar, eluant B1)
concentrationconcentrated by evaporation
filtrationthe solid portion is filtered off with suction
dry with materialdried in a high vacuμmand the title compound
customis obtained in the form of a white powder

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-79f9873b91664b99a9401d57baceb145
来源数据集: uspto-grants-1986_09
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04613676
来源说明: uspto-grants-1986_09

反应 SMILES

[NH:1]([C:38]([O:40][CH2:41][C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1)=[O:39])[C@H:2]([C:10]([NH:12][C@H:13]([C:20]([NH:22][C@H:23]([C:28]([NH:30][C@H:31]([C:35]([OH:37])=[O:36])[CH:32]([CH3:34])[CH3:33])=[O:29])[CH2:24][CH:25]([CH3:27])[CH3:26])=[O:21])[CH2:14][C:15]1[N:19]=[CH:18][NH:17][CH:16]=1)=[O:11])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C([O:52][C:53]([CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][NH-:62])=[O:54])(C)(C)C>FC(F)(F)C(O)=O>[NH:1]([C:38]([O:40][CH2:41][C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1)=[O:39])[C@H:2]([C:10]([NH:12][C@H:13]([C:20]([NH:22][C@H:23]([C:28]([NH:30][C@H:31]([C:35]([OH:37])=[O:36])[CH:32]([CH3:34])[CH3:33])=[O:29])[CH2:24][CH:25]([CH3:27])[CH3:26])=[O:21])[CH2:14][C:15]1[N:19]=[CH:18][NH:17][CH:16]=1)=[O:11])[CH2:3][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.[C:53]([CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][NH-:62])([OH:54])=[O:52]