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ChemicalBook CAS DataBase List THIENO[3,2-B]THIOPHENE-2-CARBOXYLIC ACID
1723-27-9

THIENO[3,2-B]THIOPHENE-2-CARBOXYLIC ACID synthesis

8synthesis methods
-

Yield:1723-27-9 100%

Reaction Conditions:

with lithium hydroxyde monohydrate in lithium hydroxide monohydrate at 100; for 3 h;Inert atmosphere;Large scale;

Steps:

1.3

Under a nitrogen atmosphere, lithium hydroxide monohydrate (17. 8 Kg, 662.4 mol, 1.47 eq), H20 (440.0 OKg) was added to the 2000 L autoclave and stirred to dissolve the lithium hydroxide monohydrate in water. At room temperature, the intermediate 3 (95.5 ?, 449.8111 01, 1.069) was pumped into the reaction mixture, followed by 1 '(379.5 ). Heating to reflux (about 100 ° C) for 3 hours, cooling to 35 to 40 ° C and removing the tetrahydrofuran by rotary evaporation under reduced pressure under a nitrogen atmosphere Water (200 Kg) was added to the reaction vessel Controlled temperature below 20 ° C (74.6 Kg), filtered and the filter cake was washed three times with cold water (20 Kg) and centrifuged until no liquid was obtained, product 4 (146 Kg, yield 100%)..

References:

CN103172646,2016,B Location in patent:Paragraph 0108-0110

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