4-methoxybenzene-1,3-diamine

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: 4-Methoxy-benzene-1,3-diamine (D-3) was synthesized following the general scheme above starting from 1-methoxy-2,4-dinitro-benzene. Yield (quant.). HPLC ret. time 0.31 min, 10-99% CH3CN, 5 min run. Yield (quant.)

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

実験手順: 4-Methoxy-benzene-1,3-diamine (D-3) was synthesized following the general scheme above starting from 1-methoxy-2,4-dinitro-benzene. Yield (quant.). HPLC ret. time 0.31 min, 10-99% CH3CN, 5 min run. Yield (quant.)

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methyl 1-chloroisoquinoline-5-carboxylate (0.5 g, 2.26 mmol) obtained in Step (1) above was dissolved in 2-propanol (5 mL), and added with 5-amino-p-methoxyaniline (0.33 g, 2.74 mmol) at room temperature. The reaction solution was sealed and stirred for 4 hours or more at 90° C. The reaction mixture was cooled to room temperature, and the solvent was distilled under reduced pressure. The concentrated solid was added with diethyl ether, the solid thus obtained was filtered under reduced pressure. The resulting solid was dried with warm wind in an oven (40° C.) for 3 hours or more to obtain the title compound (0.42 g, 61%). The reaction solution was sealed The reaction mixture was cooled to room temperature the solvent was distilled under reduced pressure The concentrated solid was added with diethyl ether the solid thus obtained was filtered under reduced pressure The resulting solid was dried with warm wind in an oven (40° C.) for 3 hours or more

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

実験手順: Other aqueous processes of acylation have been taught to yield the single desired isomer compound I where R is --CH3 and --XR1 is --COCH3, but at lower yield. German 1,543,625, Example 1, teaches the acylation of freshly-distilled 2,4-diaminoanisole with acetic anhydride in water solution, without the addition of hydrochloric acid, to give 3-amino-4-methoxyacetanilide in 75% yield before recrystallization. Publication, Board of Federal Intelligence Agency, P.B. 74 051, p. 33 teaches a similar conversion of 2,4-diaminoanisole to 2-amino-4-acetamidoanisole, in aqueous solution, with acetic anhydride, in the presence of magnesia at 65% yield. at lower yield

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

実験手順: Other aqueous processes of acylation have been taught to yield the single desired isomer compound I where R is --CH3 and --XR1 is --COCH3, but at lower yield. German 1,543,625, Example 1, teaches the acylation of freshly-distilled 2,4-diaminoanisole with acetic anhydride in water solution, without the addition of hydrochloric acid, to give 3-amino-4-methoxyacetanilide in 75% yield before recrystallization. Publication, Board of Federal Intelligence Agency, P.B. 74 051, p. 33 teaches a similar conversion of 2,4-diaminoanisole to 2-amino-4-acetamidoanisole, in aqueous solution, with acetic anhydride, in the presence of magnesia at 65% yield. at lower yield

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

実験手順: 4-Methoxy-benzene-1,3-diamine (D-3) was synthesized following the general scheme above starting from 1-methoxy-2,4-dinitro-benzene. Yield (quant.). HPLC ret. time 0.31 min, 10-99% CH3CN, 5 min run. Yield (quant.)

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

実験手順: 4-Methoxy-benzene-1,3-diamine (D-3) was synthesized following the general scheme above starting from 1-methoxy-2,4-dinitro-benzene. Yield (quant.). HPLC ret. time 0.31 min, 10-99% CH3CN, 5 min run. Yield (quant.)

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

実験手順: 4-Methoxy-benzene-1,3-diamine (D-3) was synthesized following the general scheme above starting from 1-methoxy-2,4-dinitro-benzene. Yield (quant.). HPLC ret. time 0.31 min, 10-99% CH3CN, 5 min run. Yield (quant.)

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

実験手順: 4-Methoxy-benzene-1,3-diamine (D-3) was synthesized following the general scheme above starting from 1-methoxy-2,4-dinitro-benzene. Yield (quant.). HPLC ret. time 0.31 min, 10-99% CH3CN, 5 min run. Yield (quant.)