HRID589425

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：CC(C)(C)OC(=O)[N-]CCCCCC[NH-].CCC(C)C1NC(=O)CNC(=O)C2Cc3c([nH]c4cc(O)ccc34)S(=O)CC(NC(=O)CNC1=O)C(=O)NC(CC(=O)O)C(=O)N1CC(O)CC1C(=O)NC(C(C)C(O)CO)C(=O)N2

HCID178453385

未命名化合物

PRODUCTS

生成物

结构：CCC(C)C1NC(=O)CNC(=O)C2Cc3c([nH]c4cc(O)ccc34)S(=O)CC(NC(=O)CNC1=O)C(=O)NC(CC(=O)O)C(=O)N1CC(O)CC1C(=O)NC(C(C)C(O)CO)C(=O)N2.[NH-]CCCCCC[NH-]

HCID131734463

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

4.54 mg (4.05 μmol) β-Amanitin-(t-butyloxy-carbonyl)-hexamethylenediamide (I) was stirred at room temperature in 250 μl trifluoroacetic acid. After 2 minutes the excess TFA was evaporated at 20° C. and the remaining solid coevaporated 2 times with 1 ml acetonitrile and methanol. The crude amine was dissolved in 1000 μl dmso and prified on a LaPrep-HPLC: column: Kromasil 100-C18, 10 μm, 250×20 mm, with methanol/water (0.05% TFA), flow: 26 ml/min, detection at λ295 nm. Solvent A: 95% water: 5% methanol 0.05% trifluoroacetic acid. Solvent B: 10% water: 90% methanol 0.05% trifluoroacetic acid. Gradient: 0-5 min 100% A; 5-20 25 min 0% A; 25-27 min 100% A; 27-35 min 100% A. The fractions with the same retention time were collected and the solvents evaporated.

WORKUP

后处理

customAfter 2 minutes the excess TFA was evaporated at 20° C.
dissolutionThe crude amine was dissolved in 1000 μl dmso
custom0-5 min 100% A
custom5-20 25 min 0% A
custom25-27 min 100% A
custom27-35 min 100% A
customThe fractions with the same retention time were collected
customthe solvents evaporated

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-e56c075962344b6784d7c85b76c6bc3c
来源数据集: uspto-grants-2016_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09233173B2
来源说明: uspto-grants-2016_01

反应 SMILES

[CH3:1][CH2:2][CH:3]([CH:5]1[NH:27][C:25](=[O:26])[CH2:24][NH:23][C:21](=[O:22])[CH:20]2[NH:28][C:29]([CH:31]([CH:51]([CH:53]([OH:56])[CH2:54][OH:55])[CH3:52])[NH:32][C:33]([CH:35]3[N:39]([C:40]([CH:42]([CH2:46][C:47]([OH:49])=[O:48])[NH:43][C:44](=[O:45])[CH:13]([CH2:14][S:15]([C:17]4[NH:59][C:58]5[CH:60]=[C:61]([OH:64])[CH:62]=[CH:63][C:57]=5[C:18]=4[CH2:19]2)=[O:16])[NH:12][C:10](=[O:11])[CH2:9][NH:8][C:6]1=[O:7])=[O:41])[CH2:38][CH:37]([OH:50])[CH2:36]3)=[O:34])=[O:30])[CH3:4].C(OC([N-:72][CH2:73][CH2:74][CH2:75][CH2:76][CH2:77][CH2:78][NH-:79])=O)(C)(C)C>FC(F)(F)C(O)=O>[CH3:1][CH2:2][CH:3]([CH:5]1[NH:27][C:25](=[O:26])[CH2:24][NH:23][C:21](=[O:22])[CH:20]2[NH:28][C:29]([CH:31]([CH:51]([CH:53]([OH:56])[CH2:54][OH:55])[CH3:52])[NH:32][C:33]([CH:35]3[N:39]([C:40]([CH:42]([CH2:46][C:47]([OH:49])=[O:48])[NH:43][C:44](=[O:45])[CH:13]([CH2:14][S:15]([C:17]4[NH:59][C:58]5[CH:60]=[C:61]([OH:64])[CH:62]=[CH:63][C:57]=5[C:18]=4[CH2:19]2)=[O:16])[NH:12][C:10](=[O:11])[CH2:9][NH:8][C:6]1=[O:7])=[O:41])[CH2:38][CH:37]([OH:50])[CH2:36]3)=[O:34])=[O:30])[CH3:4].[NH-:72][CH2:73][CH2:74][CH2:75][CH2:76][CH2:77][CH2:78][NH-:79]