Yield:-

Reaction Conditions:

Stage #1:4-(2,2-diethoxy-ethyl)-morpholine with hydrogenchloride;water at 80; for 2 h;
Stage #2: with sodium hydrogencarbonate in water; pH=~ 10 at 20;

Steps:

28
Preparation of Intermediate 8Intermediate 7 Intermediate 8; [0209] A solution of Intermediate 7 (600 mg, 2.95 mmol) dissolved in concentrated aqueous HCI (4 mL) was stirred at 80 °C for 2 h. The reaction mixture was cooled to RT, made alkaline (pH ~10) with saturated aqueous NaHC0₃ (20 mL) and the resulting solution was extracted with DCM (3 x 50 mL). The combined organic layers were washed with water (50 mL), brine (30 mL), dried over Na₂S0₄, filtered and concentrated in vacuo to obtain crude Intermediate 8 (340 mg) as a colorless oil which was used without additional purification. TLC: 60% EtOAc in hexane: R_f: 0.30.

References:

VERSEON, INC.;SHORT, Kevin, Michael;PHAM, Son, Minh;WILLIAMS, David, Charles;DATTA, Somalee WO2011/126903, 2011, A2 Location in patent:Page/Page column 79

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