HRID1982306

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID222

Ammonia gas

H3N

2 次

HCID6422

未命名化合物

结构：CC[C@H](C)[C@H](NC(=O)C[C@H](O)[C@H](CC(C)C)NC(=O)[C@H](Cc1c[nH]cn1)NC(=O)[C@H](Cc1ccccc1)NC(=O)[C@@H]1CCCN1C(=O)[C@H](Cc1c[nH]cn1)NC(=O)[C@@H]1CCCN1)C(=O)N[C@@H](Cc1c[nH]cn1)C(=O)N[C@@H](CCCCN)C(=O)OC

HCID178455895

未命名化合物

PRODUCTS

生成物

结构：CC[C@H](C)[C@H](NC(=O)C[C@H](O)[C@H](CC(C)C)NC(=O)[C@H](Cc1c[nH]cn1)NC(=O)[C@H](Cc1ccccc1)NC(=O)[C@@H]1CCCN1C(=O)[C@H](Cc1c[nH]cn1)NC(=O)[C@@H]1CCCN1)C(=O)N[C@@H](Cc1c[nH]cn1)C(=O)N[C@@H](CCCCN)C(=O)O

HCID178455894

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID962

Water

H2O

PROCEDURE

实验过程

370 mg of H-Pro-His-Pro-Phe-His-Sta-Ile-His-Lys-OMe×5 TFA are dissolved in 8 ml of H2O. The pH value is increased to 5.0 with 0.3N NH3, whereupon 40 μl of a 1% aqueous solution of trypsin are added and the pH value is maintained constant by means of a pH stat with the addition of 0.3N NH3. The absorption of base is complete after approximately 40 minutes. 1 ml of glacial acetic acid is added, the whole is heated for 2 minutes in a boiling water bath, concentrated to approximately 3 ml and lyophilised. The residue is dissolved in 3 ml of 0.05N AcOH, converted into the acetate by slowly being filtered through a column (φ=1 cm, length=10 cm) of weakly basic ion exchanger (Merck No. II) in acetate form, and the eluate is again lyophilised, yielding H-Pro-His-Pro-Phe-His-Sta-Ile-His-Lys-OH×AcOH in the form of amorphous white powder; Rf (D)=0.12; Rf (K)=0.14.

WORKUP

后处理

additionare added
customThe absorption of base
addition1 ml of glacial acetic acid is added
temperaturethe whole is heated for 2 minutes in a boiling water bath
concentrationconcentrated to approximately 3 ml
dissolutionThe residue is dissolved in 3 ml of 0.05N AcOH
filtrationby slowly being filtered through a column (φ=1 cm, length=10 cm) of weakly basic ion exchanger (Merck No. II) in acetate form

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-3ce72958219e467fb061df3308b4e814
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]1[CH2:85][CH2:84][CH2:83][C@H:2]1[C:3]([NH:5][C@H:6]([C:13]([N:15]1[CH2:82][CH2:81][CH2:80][C@H:16]1[C:17]([NH:19][C@H:20]([C:28]([NH:30][C@H:31]([C:38]([NH:40][C@H:41]([C@H:46]([CH2:48][C:49]([NH:51][C@H:52]([C:57]([NH:59][C@H:60]([C:67]([NH:69][C@H:70]([C:76]([O:78]C)=[O:77])[CH2:71][CH2:72][CH2:73][CH2:74][NH2:75])=[O:68])[CH2:61][C:62]1[N:66]=[CH:65][NH:64][CH:63]=1)=[O:58])[C@H:53]([CH2:55][CH3:56])[CH3:54])=[O:50])[OH:47])[CH2:42][CH:43]([CH3:45])[CH3:44])=[O:39])[CH2:32][C:33]1[N:37]=[CH:36][NH:35][CH:34]=1)=[O:29])[CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:18])=[O:14])[CH2:7][C:8]1[N:12]=[CH:11][NH:10][CH:9]=1)=[O:4].C(O)(C(F)(F)F)=O.N>O>[NH:1]1[CH2:85][CH2:84][CH2:83][C@H:2]1[C:3]([NH:5][C@H:6]([C:13]([N:15]1[CH2:82][CH2:81][CH2:80][C@H:16]1[C:17]([NH:19][C@H:20]([C:28]([NH:30][C@H:31]([C:38]([NH:40][C@H:41]([C@H:46]([CH2:48][C:49]([NH:51][C@H:52]([C:57]([NH:59][C@H:60]([C:67]([NH:69][C@H:70]([C:76]([OH:78])=[O:77])[CH2:71][CH2:72][CH2:73][CH2:74][NH2:75])=[O:68])[CH2:61][C:62]1[N:66]=[CH:65][NH:64][CH:63]=1)=[O:58])[C@H:53]([CH2:55][CH3:56])[CH3:54])=[O:50])[OH:47])[CH2:42][CH:43]([CH3:44])[CH3:45])=[O:39])[CH2:32][C:33]1[N:37]=[CH:36][NH:35][CH:34]=1)=[O:29])[CH2:21][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)=[O:18])=[O:14])[CH2:7][C:8]1[N:12]=[CH:11][NH:10][CH:9]=1)=[O:4]