반응 #7015

ord-6f19733c657e4b04b7ed2ac578424390

반응 방정식

COCCNCc1nnc(C2CCN(c3ccccn3)CC2)n1Cc1ccccc1
amine
COCCNCc1nnc(C2CCN(c3ccccn3)CC2)n1Cc1ccccc1
[4-Benzyl-5-(3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl)-4H-[1,2,4]triazol-3-ylmethyl]-(2-methoxy-ethyl)-amine
C=O
formaldehyde
CC(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+]
sodium triacetoxyborohydride
COCCN(C)Cc1nnc(C2CCN(c3ccccn3)CC2)n1Cc1ccccc1
title compound
COCCN(C)Cc1nnc(C2CCN(c3ccccn3)CC2)n1Cc1ccccc1
[4-Benzyl-5-(3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl)-4H-[1,2,4]triazol-3-ylmethyl]-(2-methoxy-ethyl)-methyl-amine

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture was partitioned between dichloromethane and aqueous sodium carbonate solution
  2. 2
    기타the layers separated
  3. 3
    건조The organic phase was dried (MgSO4)
  4. 4
    기타evaporated under reduced pressure
  5. 5
    기타the product triturated from ether

실험 절차

The amine from example 43 (50 mg, 0.12 mmol), formaldehyde (37% aq, 40 μl, 0.49 mmol) and sodium triacetoxyborohydride (51 mg, 0.24 mmol) in dichloromethane (1 ml) was stirred vigorously at room temperature for 21 hours. The reaction mixture was partitioned between dichloromethane and aqueous sodium carbonate solution, and the layers separated. The organic phase was dried (MgSO4), evaporated under reduced pressure, and the product triturated from ether to afford the title compound as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084145B2uspto-grants-2006_08