반응 #1882128

반응 방정식

N-[2-(2-nitro-benzenesulfonylamino)-ethyl]-N-[(thymin-1-yl)-acetyl]-glycine

N-mehtyl morpholine

water

→

compound

수율 98.0%

1-(2-Nitro-benzenesulfonyl)-4-[(thymin-1-yl)-acetyl]-piperazin-2-one

수율 98.0%

용매

THF

반응 조건

후처리

1. 1
   기타to precipitate solid
2. 2
   여과The solid was filtered off
3. 3
   세척washed with water
4. 4
   기타dried in vacuo

실험 절차

To a solution of N-[2-(2-nitro-benzenesulfonylamino)-ethyl]-N-[(thymin-1-yl)-acetyl]-glycine (469 mg, 1.0 mmol) and N-mehtyl morpholine (330 μL, 3 mmol) in THF (10 mL) was added isobutylchloroformatre (205 mg, 1.5 mmol) at −20° C. The reaction mixture was allowed to warm to 0° C. for a period of 1 h. Then water (10 mL) was added to the reaction mixture to precipitate solid. The solid was filtered off, washed with water, dried in vacuo to give the tiltled compound (442 mg, 98%). 1H-NMR (500 MHz; DMSO-d6) δ 11.32 (s, 0.6H), 11.30 (s, 0.4H), 8.35 (m, 1H), 8.12 (dd, 1H), 8.04˜7.96 (m, 2H), 7.35 (s, 0.6H), 7.28 (s, 0.4H), 4.67 (s, 1.2H), 4.59 (s, 0.8H), 4.41 (s, 0.8H), 4.27 (s, 1.2H), 4.04 (m, 1.2H), 3.95 (m, 1.2H), 3.90˜3.85 (m, 1.6H), 1.75 (s, 3H).

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