Trifluoroacetic acid methylene chloride → HCID 25159797, compound
Reaction equation
C(OC([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][C@H:13]([NH:21][C:22]([NH:24][C@@H:25]([C:33](=[O:40])[NH:34][CH2:35][CH2:36][CH:37]([CH3:39])[CH3:38])[CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:23])[C:14]([O:16]C(C)(C)C)=[O:15])=O)(C)(C)C.[Cl:41]CCl.C(O)(C(F)(F)F)=O>>[ClH:41].[NH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C@H:13]([NH:21][C:22]([NH:24][C@@H:25]([C:33](=[O:40])[NH:34][CH2:35][CH2:36][CH:37]([CH3:38])[CH3:39])[CH2:26][C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)=[O:23])[C:14]([OH:16])=[O:15]Participants
3
Procedure
The product from Example 1c) (0.500 g, 0.889 mmol) was dissolved in dichloromethane/TFA (10 ml, 1:1, v/v) and stirred at RT for 2 h. The solution was concentrated and purified by preparative HPLC. The combined product fractions were mixed with 2N HCl, concentrated and freeze dried.
Workup
- concentrationThe solution was concentrated
- custompurified by preparative HPLC
- additionThe combined product fractions were mixed with 2N HCl
- concentrationconcentrated
- customfreeze dried
Sources & evidence
- ORD record
- ord-7069295ac2b548b8ad3d9baa27789c74
- Source dataset
- uspto-grants-2013_03
- Patent number
- US08389764B2
Reaction notes
Loading…