تفاعل #68335

معادلة التفاعل

ethyl4-iodo-3nitrobenzoate

Compound 30

ethyl4-iodo-3nitrobenzoate

tin(II) chloride

→

title compound

Ethyl 3-Amino-4-iodobenzoate

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىReaction
2. 2
   درجة الحرارةcooled to 25° C.
3. 3
   أخرىquenched with NaHCO3(S)
4. 4
   ترشيحfiltered off white solid
5. 5
   تركيزorganic layer was concentrated in vacuo
6. 6
   أخرىThe residue was purified by chromatography on silica gel (0→50% EtOAc-hexanes)

الإجراء التجريبي

To a solution of ethyl4-iodo-3nitrobenzoate (Compound 30, 9.45 g, 29.4 mmol) in ethyl acetate (200 ml) and tin(II) chloride dehydrate (33.1 g, 147 mmol). Reaction was heated to 85° C. for 1 h, cooled to 25° C., quenched with NaHCO3(S), filtered off white solid, and then organic layer was concentrated in vacuo. The residue was purified by chromatography on silica gel (0→50% EtOAc-hexanes) to yield the title compound as a light yellow solid.

المصدر