Hydrochloric Acid → HCID 58419173, compound

HRID 1803725Notes

Reaction equation

[Cl:1][C:2]([F:42])([O:21][C:22]([F:41])([F:40])[C:23]([F:39])([O:28][C:29]([F:38])([F:37])[C:30]([F:36])([F:35])[C:31]([F:34])([F:33])[F:32])[C:24]([F:27])([F:26])[F:25])[C:3]([F:20])([F:19])[O:4][C:5]1[CH:14]=[C:13]([C:15]([O:17]C)=[O:16])[CH:12]=[CH:11][C:6]=1[C:7]([O:9]C)=[O:8].[OH-].[K+].Cl>O>[Cl:1][C:2]([F:42])([O:21][C:22]([F:40])([F:41])[C:23]([F:39])([O:28][C:29]([F:38])([F:37])[C:30]([F:36])([F:35])[C:31]([F:34])([F:33])[F:32])[C:24]([F:25])([F:26])[F:27])[C:3]([F:19])([F:20])[O:4][C:5]1[CH:14]=[C:13]([C:15]([OH:17])=[O:16])[CH:12]=[CH:11][C:6]=1[C:7]([OH:9])=[O:8]

Participants

Conditions

Temperature: 25 °C

Procedure

Dimethyl 2-(2-chloro-1,1,2-trifluoro-2-(1,1,2,3,3,3-hexafluoro-2-(perfluoropropoxy)propoxy)ethoxy)terephthalate as prepared in Example 3 (10.00 g, 0.0148 mol) was added to a solution of water (100 mL) and potassium hydroxide (KOH, 8.0 g) in a reaction flask. The resulting solution in the reaction flask was heated to reflux overnight, cooled to room temperature (about 25° C.) and then acidified by adding concentrated HCl to the reaction flask to achieve a pH of ˜1, determined by the formation of a precipitate in the reaction flask. The resulting precipitate was filtered and dried under vacuum. NMRs of this precipitate showed the desired material, 2-(2-chloro-1,1,2-trifluoro-2-(1,1,2,3,3,3-hexafluoro-2-(perfluoropropoxy)propoxy)ethoxy)terephthalic acid.

Workup

temperatureThe resulting solution in the reaction flask was heated
temperatureto reflux overnight
filtrationThe resulting precipitate was filtered
customdried under vacuum

Sources & evidence

ORD record: ord-179e56def96b40f79877b718d6db4c38
Source dataset: uspto-grants-2013_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08350099B2

Reaction notes

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