反応 #1060904

ord-9d3134bdfaae4dde982fa1a852abdee2

反応方程式

CC(C)(C)OC(=O)OC(=O)[O-]
tert-butyl dicarbonate
NCCCNCCCN
3,3'-diaminodipropylamine
O
water
CC(C)(C)OC(=O)NC(CCN)CCCN
expected product
収率 44.7%
CC(C)(C)OC(=O)NC(CCN)CCCN
N-(tert-butoxycarbonyl)-(3-amino propyl)-1,3-propanediamine
収率 44.7%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他by decanting
  2. 2
    その他evaporation to dryness
  3. 3
    その他The residue was chromatographed on silica (eluant; methanol-ammonia (98-2))

実験手順

A solution of 33 g of tert-butyl dicarbonate in 200 ml of methylene chloride was added at 5° C. to a solution of 39.3 g of 3,3'-diaminodipropylamine in 300 ml of methylene chloride and after stirringf or 16 hours at 20° C., water was added, followed by decanting and evaporation to dryness. The residue was chromatographed on silica (eluant; methanol-ammonia (98-2)) to obtain 15.5 g of the expected product which was used as is for the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05064861uspto-grants-1991_11