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ChemicalBook CAS DataBase List 2-(2-CHLORO-ACETYLAMINO)-5,6,7,8-TETRAHYDRO-4H-CYCLOHEPTA[B]THIOPHENE-3-CARBOXYLIC ACID ETHYL ESTER
76981-88-9

2-(2-CHLORO-ACETYLAMINO)-5,6,7,8-TETRAHYDRO-4H-CYCLOHEPTA[B]THIOPHENE-3-CARBOXYLIC ACID ETHYL ESTER synthesis

3synthesis methods
-

Yield:76981-88-9 37%

Reaction Conditions:

with triethylamine in diethyl ether at 20; for 4 h;

Steps:

Preparation of 12

Compound 11 (2.0 g, 8.36 mmol) is dissolved in diethyl ether (60 mL) and treated with triethyl amine (1.3 mL, 9.2 mmol). To this mixture, chloroacetyl chloride (1.04 g, 9.2 mmol) dissolved in diethyl ether (5 mL) is added dropwise at room temperature. This mixture is stirred for 4 hours at room temperature. The mixture is partitioned between water (30 mL) and ether (30 mL). The organic layer is separated, dried [(MGS04)] and concentrated. The residue is subjected to chromatography by elution with [5%] ethyl acetate in heptane to give the desired product as a white solid (0.965 g, 37% yield). Physical characteristics: MS (ES-) for [M/Z] 314 (M-H) [+.]

References:

WO2003/101979,2003,A1 Location in patent:Page 22

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