Allylamine → 8-Azabicyclo[4.3.0]non-2-ene

반응식

[NH2:1][CH2:2][CH:3]=[CH2:4].Br[CH2:6]/[CH:7]=[CH:8]/[CH:9]=[CH2:10]>>[CH:9]12[CH2:10][NH:1][CH2:2][CH:3]1[CH2:4][CH2:6][CH:7]=[CH:8]2

참가 물질

반응물 2

HCID 7853Allylamine

HCID 5365559(3E)-5-Bromo-1,3-pentadiene

생성물 1

HCID 123867678-Azabicyclo[4.3.0]non-2-ene

실험 절차

The starting material is 228 g (4.0 mol) of 1-amino-2-propene. 58.8 g (0.4 mol) of (E)-1-bromo-2,4-pentadiene (title compound of Example A.1.) are added dropwise, with stirring. The internal temperature is kept in the range 20°-30° C. by cooling. The reaction mixture is stirred for 5 h at room temperature and concentrated at 150 mbar. A solution of 20 g (0.5 mol) of sodium hydroxide in 200 ml of water is added, the mixture is extracted with twice 100 ml of methylene chloride, the extracts are dried over sodium sulphate, 0.1 g of 4-hydroxyanisole is added and the mixture is concentrated and distilled at 40 mbar. The distillate is stabilized by the addition of 10-20 ppm of 4-hydroxyanisole.

출처 및 근거

ORD 기록: ord-50bbb079971547c88c57f747d7d39c06
출처 데이터셋: uspto-grants-1996_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05508278

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