Trifluoroacetic acid → HCID 66614942, compound

HRID 2046037Notes

Reaction equation

HRID 2046037 reaction equation
[CH2:1]([C:9]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:20][CH2:19][N:18](C(OC(C)(C)C)=O)[CH2:17][CH2:16]2)=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[C:28]([OH:34])([C:30]([F:33])([F:32])[F:31])=[O:29]>C(Cl)Cl.CCO>[C:28]([OH:34])([C:30]([F:33])([F:32])[F:31])=[O:29].[CH2:1]([C:9]1[CH:10]=[CH:11][C:12]([N:15]2[CH2:16][CH2:17][NH:18][CH2:19][CH2:20]2)=[CH:13][CH:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

Participants

6

Reactant 2

HCID 6422Trifluoroacetic acidHCID 86660604HCID 86660604, compound

Product 2

HCID 6422Trifluoroacetic acidHCID 66614942HCID 66614942, compoundYield 100%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 6344DichloromethaneSolvent

Procedure

A solution of the product of Step C (0.06 g; 0.16 mmol) in 60% TFA in CH2Cl2 (2 ml) was stirred for 15 min at room temperature and the mixture was diluted to 5 ml with EtOH and evaporated to dryness under reduced pressure and kept in vacuo for 1 h, to give a TFA salt of the title compound (0.07 g; 100%). 1H-NMR (CDCl3) 9.5 (broad s, 2H); 7.29 (m, 4H); 3.8-3.16 (m, 8H); 2.6 (t, 2H, J=8 Hz); 1.58 (m, 2H); 1.26 (m, 10H); 0.86 (t, 3H, J=6.9 Hz).

Workup

  1. customevaporated to dryness under reduced pressure

Sources & evidence

ORD record
ord-d614413db59d4d1ab2a66eb5ed55fef9
Source dataset
uspto-grants-2013_11
Patent number
US08592399B2

Reaction notes

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