1.1
Reagents:
N,N-Dimethylaniline
Solvents:
Dichloromethane
;
1 h, rt; 2 h, 30 - 35 °C; cooled
1.2
Reagents:
Water
;
cooled
2.1
Reagents:
Sodium hydroxide
Solvents:
Methanol
,
Water
;
rt; 3.5 h, 35 °C; 0.5 h, 35 °C; 35 °C → 5 °C
2.2
Reagents:
Hydrochloric acid
Solvents:
Water
;
pH 2.8 - 3.0, 0 - 5 °C; 0.5 h, 0 - 5 °C
3.1
Reagents:
Triethylamine
,
Triethyl phosphite
Solvents:
Acetonitrile
;
3 h, rt