1-iodo-3-(trifluoromethoxy)benzene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The title compound was prepared from (R)-2-methyl-4-(3-piperidin-1-yl-propyl)-[1,4]diazepan-5-one (Example 39E) and 1-iodo-3-trifluoromethoxy-benzene in analogy to example 33. MS: 414.4 (MH+).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The title compound was prepared from (R)-2-methyl-4-(3-piperidin-1-yl-propyl)-[1,4]diazepan-5-one (Example 39E) and 1-iodo-3-trifluoromethoxy-benzene in analogy to example 33. MS: 414.4 (MH+).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The title compound was prepared from 4-[3-((S)-4-hydroxy-6-aza-spiro[2.5]oct-6-yl)-propyl]-[1,4]diazepan-5-one and 1-iodo-3-trifluoromethoxy-benzene in analogy to example 33. MS: 442.3 (MH+).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The title compound was prepared from 4-(3-piperidin-1-yl-propyl)-[1,4]diazepan-5-one (Example 33B) and 1-iodo-3-trifluoromethoxy-benzene in analogy to example 33. MS: 400.2 (MH+).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-iodo-3-(trifluoromethoxy)benzene (5.00 g), copper(I) iodide (66.3 mg), triphenylphosphine (228 mg), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (360 mg), propargyl alcohol (1.13 ml), diisopropylethylamine (12.1 ml) and tetrahydrofuran (100 ml) was stirred at room temperature for 15 hr. The reaction mixture was added to brine, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-80:20) to give the object product (3.28 g) as a brown oil. the mixture was extracted with ethyl acetate washed with saturated brine dried over anhydrous magnesium sulfate The solvent was evaporated under reduced pressure The residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-80:20)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The title compound was prepared in analogy to intermediate 6A by reaction of 3,5-Dimethyl-1H-pyrazole-4-carboxylic acid ethyl ester (2 g, 12 mmol) with 3-trifluoromethoxyiodobenzene (6.7 g, 14 mmol) affording the desired product (2.9 g, 73%) as a colourless liquid. MS: 329.2 (MH1).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The title compound was prepared in analogy to intermediate 6A by reaction of 3,5-Dimethyl-1H-pyrazole-4-carboxylic acid ethyl ester (2 g, 12 mmol) with 3-trifluoromethoxyiodobenzene (6.7 g, 14 mmol) affording the desired product (2.9 g, 73%) as a colourless liquid. MS: 329.2 (MH1).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In analogy to the procedures described in example 1F], 1-iodo-3-trifluoromethoxy-benzene and pent-4-yn-1-ol gave the title compound as a red liquid.