반응 #1563912

ord-75859f3919c641128339ff193cf6922a

반응 방정식

CC(=O)NCc1cc2c(cc1I)OCO2
N-((6-Iodobenzo[d][1,3]dioxol-5-yl)methyl)acetamide
NCc1cc2c(cc1I)OCO2
(6-iodobenzo[d][1,3]dioxol-5-yl)methanamine
수율 85.0%

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Solvent was removed
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in water
  3. 3
    여과filtered

실험 절차

N-((6-Iodobenzo[d][1,3]dioxol-5-yl)methyl)acetamide (2.4 g, 7.5 mmol) was added to methanolic hydrochloric acid solution (4 N) (60 mL). The mixture was stirred at 80° C. overnight. Solvent was removed and the residue was dissolved in water, adjusted to PH7 with 10% NaHCO3, filtered to obtain (6-iodobenzo[d][1,3]dioxol-5-yl)methanamine as a yellow solid (1.76 g, 85%). LC-MS: 278 [M+1]+. 1H-NMR (DMSO-d6): δ 1.88 (s, 2H), 3.57 (s, 2H), 6.02 (s, 2H), 7.13 (s, 1H), 7.33 (s, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09402832B2uspto-grants-2016_08