반응 #1106679

ord-d2142af620fa4a2c8bdc18213fc7bd03

반응 방정식

NCC1COc2ccccc2O1
Racemic 2,3-dihydro-1,4-benzdioxin-2-ylmethylamine
NS(N)(=O)=O
sulfamide
NS(=O)(=O)NCC1COc2ccccc2O1
title compound
NS(=O)(=O)NCC1COc2ccccc2O1
N-(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethyl)-sulfamide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 2 h
  2. 2
    여과a small amount of solid was filtered
  3. 3
    기타The filtrate was evaporated in vacuo
  4. 4
    기타the residue was purified
  5. 5
    기타to yield a white solid
  6. 6
    기타The solid was recrystallized from DCM

실험 절차

Racemic 2,3-dihydro-1,4-benzdioxin-2-ylmethylamine (4.4 g, 26 mmol) and sulfamide (5.1 g, 53 mmol) were combined in 1,4 dioxane (100 mL) and refluxed for 2 h. The reaction was cooled to room temperature and a small amount of solid was filtered and discarded. The filtrate was evaporated in vacuo and the residue was purified using flash column chromatography (DCM:Methanol-10:1) to yield a white solid. The solid was recrystallized from DCM to yield the title compound as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08716231B2uspto-grants-2014_05