反応 #4029292
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-4944ca0c6b254321b14ddabafcfea167表示可能な構造データがありません
C1=CC=C(C(=C1)OC(F)F)OC(F)F製品情報
1,2-bis(difluoromethoxy)benzene (CAS 27691-14-1) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 2769568
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
7 反応 · 7 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-4944ca0c6b254321b14ddabafcfea167反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 15 g of 1,2-bis(difluoromethoxy)-benzene and 15 ml of 100% strength nitric acid in 150 ml of dichloromethane is stirred at room temperature for 7 hours. The mixture is neutralized with potassium bicarbonate solution and the organic layer is separated off and chromatographed on silica gel by means of cyclohexane/ethyl acetate (4:1). 1,2-Bis-(Difluoromethoxy)-4-nitro-benzene is obtained. This is hydrogenated and acetylated analogously to Example 21a to give N-[3,4-bis(difluoromethoxy)-phenyl]acetamide (m.p. 81°-83° C.). Analogously to Example 21, furthermore, N-[4,5-bis(difluoromethoxy)-2-nitrophenyl]acetamide (m.p. 65°-67° C.), N-[4,5-bis(difluoromethoxy)-2-nitro]aniline (m.p. 107°-109° C.), 4,5-bis(difluoromethoxy)-1,2-phenylenediamine dihydrochloride and the title compound of m.p. 285°-287° C. (decomposition; from isopropanol) are obtained. the organic layer is separated off chromatographed on silica gel by means of cyclohexane/ethyl acetate (4:1)
ソース ID: ord-478d46b9c0304c9896aaeaeb1b279ce1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 15 g of 1,2-bis(difluoromethoxy)-benzene and 15 ml of 100% strength nitric acid in 150 ml of dichloromethane is stirred at room temperature for 7 hours. The mixture is neutralized with potassium bicarbonate solution and the organic layer is separated off and chromatographed on silica gel by means of cyclohexane/ethyl acetate (4:1). 1,2-Bis-(Difluoromethoxy)-4-nitro-benzene is obtained. This is hydrogenated and acetylated analogously to Example 21a to give N-[3,4-bis(difluoromethoxy)-phenyl]acetamide (m.p. 81°-83° C.). Analogously to Example 21, furthermore, N-[4,5-bis(difluoromethoxy)-2-nitrophenyl]acetamide (m.p. 65°-67° C.), N-[4,5-bis(difluoromethoxy)-2-nitro]aniline (m.p. 107°-109° C.), 4,5-bis(difluoromethoxy)-1,2-phenylenediamine dihydrochloride and the title compound of m.p. 285°-287° C. (decomposition; from isopropanol) are obtained. the organic layer is separated off chromatographed on silica gel by means of cyclohexane/ethyl acetate (4:1)
ソース ID: ord-478d46b9c0304c9896aaeaeb1b279ce1反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-4944ca0c6b254321b14ddabafcfea167反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 15 g of 1,2-bis(difluoromethoxy)benzene and 15 ml of 100% strength nitric acid in 150 ml of methylene chloride is stirred for 7 h at room temperature. The solution is neutralized with potassium bicarbonate solution and the organic phase is separated off. After chromatography on silica gel with cyclohexane/ethyl acetate (4:1), 1,2-bis(difluoromethoxy)-4-nitrobenzene is obtained, which is hydrogenated and acetylated analogously to Example 5a to yield N-[3,4-bis(difluoromethoxy)phenyl]-acetamide of m.p. 81°-83° C. Further reaction analogously to Example 5 gives N-[4,5-bis(difluoromethoxy)-2-nitrophenyl]-acetamide of m.p. 65°-67° C., N-[4,5-bis(difluoromethoxy)-2-nitro]-aniline of m.p. 107°-109° C., 4,5-bis(difluoromethoxy)-1,2-phenylenediamine dihydrochloride and the title compound of m.p. 285°-287° C. (decomposition; from isopropanol). the organic phase is separated off
ソース ID: ord-35dbae88066f4d32b7cf92459d93c3d9反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 15 g of 1,2-bis(difluoromethoxy)-benzene and 15 ml of 100% strength nitric acid in 150 ml of dichloromethane is stirred at room temperature for 7 hours. The mixture is neutralized with potassium bicarbonate solution and the organic layer is separated off and chromatographed on silica gel by means of cyclohexane/ethyl acetate (4:1). 1,2-Bis-(Difluoromethoxy)-4-nitro-benzene is obtained. This is hydrogenated and acetylated analogously to Example 21a to give N-[3,4-bis(difluoromethoxy)-phenyl]acetamide (m.p. 81°-83° C.). Analogously to Example 21, furthermore, N-[4,5-bis(difluoromethoxy)-2-nitrophenyl]acetamide (m.p. 65°-67° C.), N-[4,5-bis(difluoromethoxy)-2-nitro]aniline (m.p. 107°-109° C.), 4,5-bis(difluoromethoxy)-1,2-phenylenediamine dihydrochloride and the title compound of m.p. 285°-287° C. (decomposition; from isopropanol) are obtained. the organic layer is separated off chromatographed on silica gel by means of cyclohexane/ethyl acetate (4:1)
ソース ID: ord-478d46b9c0304c9896aaeaeb1b279ce1反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-4944ca0c6b254321b14ddabafcfea167PubChem References
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