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

Introduce 228 g (4.0 mol) of 1-amino-2-propene. Add dropwise with stirring 58.8 g (0.4 mol) of (E)-1-bromo-2,4-pentadiene (title compound of Example A.1.). Keep the internal temperature in a range of 20°-30° C. by means of cooling. Stir for 5 h at room temperature. Concentrate batch at 150 mbar. Add 20 g (0.5 mol) of sodium hydroxide, dissolved in 200 ml of water, extract the mixture twice using in each case 100 ml of methylene chloride, dry using sodium sulphate, add 0.1 g of 4-hydroxyanisole, concentrate and distil at 40 mbar. 10-20 ppm of 4-hydroxyanisole are added to stabilize the distillate.

후처리

additionAdd dropwise

출처 및 근거

ORD 기록: ord-09d8670013a6436586a9a5449f31f6c4
출처 데이터셋: uspto-grants-1998_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05854241

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