Ammonia → HCID 2770894, compound

HRID 1534137Notes

Reaction equation

[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH:12]([CH2:14][CH3:15])[CH3:13])[CH:2]1[O:4][CH2:3]1.[NH3:16]>O>[OH:4][CH:2]([CH2:1][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH:12]([CH2:14][CH3:15])[CH3:13])[CH2:3][NH2:16]

Participants

Conditions

Temperature: 80 °C

Procedure

A 2.5 liter autoclave is charged, at room temperature and under nitrogen blanketing, with 429 g (2.1 mol) of o-sec-butylphenyl glycidyl ether and 30.2 g of water. Then 698.5 g (41.08 mol) of ammonia gas is blown in under pressure over 5 minutes and the reaction mixture is thereafter heated to 80° C. over 2 hours. After 1 hour at 80° C., the reaction mixture is cooled to room temperature, the pressure in the system is removed and the reaction product is concentrated on a rotary evaporator at 80° C./13 mbar. Gas chromatographic analysis shows the resultant amine to be 92.5% pure. It has a viscosity of 1240 mPa·s.

Workup

temperaturethe reaction mixture is cooled to room temperature
customthe pressure in the system is removed
concentrationthe reaction product is concentrated on a rotary evaporator at 80° C./13 mbar

Sources & evidence

ORD record: ord-19a4fea213944dbab99be1b7277734c6
Source dataset: uspto-grants-1992_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05087688

Reaction notes

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