Trifluoroacetic acid → HCID 18374598, compound

HRID 2300708Notes

Reaction equation

HRID 2300708 reaction equation
[CH2:1]([C:5]1([CH2:43][CH3:44])[CH2:11][S:10](=[O:13])(=[O:12])[C:9]2[CH:14]=[CH:15][C:16]([N:18]([CH3:20])[CH3:19])=[CH:17][C:8]=2[CH:7]([C:21]2[CH:22]=[C:23]([NH:27][CH2:28][CH2:29][O:30][CH2:31][CH2:32][O:33][CH2:34][C:35]([O:37]C(C)(C)C)=[O:36])[CH:24]=[CH:25][CH:26]=2)[CH:6]1[OH:42])[CH2:2][CH2:3][CH3:4].[F:45][C:46]([F:51])([F:50])[C:47]([OH:49])=[O:48]>C(Cl)Cl>[F:45][C:46]([F:51])([F:50])[C:47]([O-:49])=[O:48].[CH2:1]([C:5]1([CH2:43][CH3:44])[CH2:11][S:10](=[O:13])(=[O:12])[C:9]2[CH:14]=[CH:15][C:16]([NH+:18]([CH3:20])[CH3:19])=[CH:17][C:8]=2[CH:7]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([NH:27][CH2:28][CH2:29][O:30][CH2:31][CH2:32][O:33][CH2:34][C:35]([OH:37])=[O:36])[CH:22]=2)[CH:6]1[OH:42])[CH2:2][CH2:3][CH3:4]

Participants

4

Reactant 2

HCID 6422Trifluoroacetic acidHCID 18342382HCID 18342382, compound

Product 1

HCID 18374598HCID 18374598, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of 90 mg of tert-butyl (2-{2-[3-(3-butyl-7-dimethylamino-3-ethyl-4-hydroxy-1,1-dioxo-2,3,4,5-tetrahydro-1H-benzo[b]thiepin-5-yl)phenylamino]ethoxy}ethoxy)acetate in 1 ml of methylene chloride and 1 ml of trifluoroacetic acid is stirred for 2 h and then concentrated. The product is purified by HPLC (Knauer Eurospher-100-10-C18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90).

Workup

  1. concentrationconcentrated
  2. customThe product is purified by HPLC (Knauer Eurospher-100-10-C18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90)

Sources & evidence

ORD record
ord-952bca2ae85a43e8b110d65d5e073d8e
Source dataset
uspto-grants-2002_12
Patent number
US06498156B2

Reaction notes

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