Trifluoroacetic acid methylene chloride → HCID 25159797, compound

HRID 1943296Notes

Reaction equation

HRID 1943296 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

  1. concentrationThe solution was concentrated
  2. custompurified by preparative HPLC
  3. additionThe combined product fractions were mixed with 2N HCl
  4. concentrationconcentrated
  5. customfreeze dried

Sources & evidence

ORD record
ord-7069295ac2b548b8ad3d9baa27789c74
Source dataset
uspto-grants-2013_03
Patent number
US08389764B2

Reaction notes

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