반응 #87527

ord-46f8d2f98c9945eb9e7783f9b2beb222

반응 방정식

Cl
HCl
COC(=O)c1ccc(N)cc1OC
methyl 4-amino-2-methoxybenzoate
O=N[O-].[Na+]
sodium nitrite
COC(=O)c1ccc(NN)cc1OC
desired product
COC(=O)c1ccc(NN)cc1OC
methyl 4-hydrazinyl-2-methoxybenzoate

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The title compound was prepared

실험 절차

The title compound was prepared according to the procedure described in step-2 of Intermediate-7 by using methyl 4-amino-2-methoxybenzoate (10.0 g, 0.055 mol), stannous chloride (31.00 g, 0.138 mmol), sodium nitrite (4.57 g, 0.066 mmol), 6 N HCl (200 mL) and water (100 mL) to afford 14.0 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 3.73 (s, 3H), 3.80 (s, 3H), 6.51 (d, J=8.4 Hz, 1H), 6.69 (s, 1H), 7.68 (d, J=8.4 Hz, 1H), 8.75 (br s, 1H), 10.28 (br hump, 2H); MS (m/z): 197.01 (M+H)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09439890B2uspto-grants-2016_09