Reaktion #560303

Reaktionsgleichung

sodium carbonate

FC(O)CF(CF3)—O—(CF2)3COF

sulfuric acid

methanol

sulfuric acid

carbon dioxide

→

CF3CFH—O—(CF2)3COOCH3

Ausbeute 56.5%

Lösungsmittel

water

diglyme

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturmaintained at that temperature for 30 minutes
2. 2
   Temperaturto cool
3. 3
   SonstigeTwo layers formed
4. 4
   Waschenthe top layer was washed with 33% sulfuric acid
5. 5
   WaschenThe reaction mixture was washed with water
6. 6
   workup.DISTILLATIONdistilled at 52° C. at 15 mmHg (2.0×103 Pa)

Vorschrift

FC(O)CF(CF3)—O—(CF2)3COF (503 grams, 1.4 mole), prepared as described in U.S. Pat. App. Pub. No. 2004/0116742, was added over a period of two hours to a stirred mixture of sodium carbonate (387 grams, 3.7 moles) and diglyme (650 grams) at 78° C. The reaction liberated carbon dioxide gas. Distilled water (35 grams, 1.9 mole) was added at 85° C., and then the reaction mixture was heated to 165° C. and maintained at that temperature for 30 minutes. The reaction was allowed to cool, and sulfuric acid (250 grams, 2.6 moles) in 1250 grams of water was added. Two layers formed, and the top layer was washed with 33% sulfuric acid and then esterified at 65° C. with methanol (200 grams, 6.3 moles) and concentrated sulfuric acid (200 grams, 2.0 moles). The reaction mixture was washed with water and distilled at 52° C. at 15 mmHg (2.0×103 Pa) to give 258 grams of CF3CFH—O—(CF2)3COOCH3.

Quelle