Reaktion #1892977

Reaktionsgleichung

Morpholine

2,4-dichlorothieno[2,3-d]pyrimidine

2,4-Dichlorothieno[2,3-d]pyrimidine

→

morpholine

Ausbeute 88.3%

4-(2-chlorothieno[2,3-d]pyrimidin-4-yl)morpholine

Ausbeute 88.3%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthe resulting slurry was filtered
2. 2
   Waschenrinsed with water (500 ml)
3. 3
   SonstigeThe cake was dried in vacuum oven at 55° C. for 24 hours

Vorschrift

Morpholine (85.1, 0.977 mol, 2.2 equiv.) was added to a solution of 2,4-dichlorothieno[2,3-d]pyrimidine 17 (91 g, 0.444 mol, 1.0 equiv.). The reaction mixture was stirred at ambient temperature for 1 h and the resulting slurry was filtered, rinsed with water (500 ml). The cake was dried in vacuum oven at 55° C. for 24 hours to give 442-chlorothieno[2,3-d]pyrimidin-4-yl)morpholine 18 as an off-white solid (100.3 g, 88% yield). 1H NMR (400 MHz, DMSO-d6) δ 3.736 (t, J=4.8 Hz, 4H), δ 3.897 (t, J=5.2 Hz, 4H), δ 7.658 (d, J=6.4 Hz, 1H), δ 7.682 (t, J=6.4 Hz, 4H δ). LCMS (ESI pos) m/e 257 (M+1).

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