Dichloroacetyl chloride → HCID 4158166, 화합물

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[N+:1]([C:4]1[O:8][C:7]([CH:9]=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].[Cl:11][CH:12]([Cl:16])C(Cl)=O.C(N(CC)CC)C>C1C=CC=CC=1>[Cl:11][C:12]([Cl:16])=[CH:9][C:7]1[O:8][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1

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실험 절차

To a stirred mixture of 14.1 g of 5-nitro-2-furaldehyde and 22.1 g of dichloroacetyl chloride in 300 ml of benzene was added dropwise at 25°-30° over a 30-minute period a solution of 15.2 g of triethylamine in 50 ml of benzene. The mixture then was stirred at 25°-30° for an additional 30 minutes and then for 90 minutes at reflux. After cooling, the mixture was filtered and the filtrate was washed and dried, concentrated under reduced pressure and Claisen distilled to give a liquid product, b.p.: 88°-98° at 0.3 torr. (mainly 90°-95°). This material was crystallized from acetone/petroleum ether to give 1 as a light yellow solid, m.p.: 74°-75°.