Hydrochloric Acid → N-[2-(2-ethoxyethoxy)-phenyl-sulfonyl]-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)-urea
反応式
O([C:8]([NH:10][C:11]1[N:16]=[C:15]([O:17][CH:18]([F:20])[F:19])[CH:14]=[C:13]([CH3:21])[N:12]=1)=[O:9])C1C=CC=CC=1.[CH2:22]([O:24][CH2:25][CH2:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[S:34]([NH2:37])(=[O:36])=[O:35])[CH3:23].N12CCCCC1C=NCCC2.Cl>C(#N)C.O.C(OCC)(=O)C>[CH2:22]([O:24][CH2:25][CH2:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[S:34]([NH:37][C:8]([NH:10][C:11]1[N:16]=[C:15]([O:17][CH:18]([F:19])[F:20])[CH:14]=[C:13]([CH3:21])[N:12]=1)=[O:9])(=[O:35])=[O:36])[CH3:23]参加物
8
反応物 4
生成物 1
試薬・触媒・溶媒 3
実験手順
A solution of 3.5 g of 2-phenoxycarbonylamino-4-difluoromethoxy-6-methyl-pyrimidine (crude product) and 2.9 g of 2-(ethoxy-ethoxy)-benzenesulfonamide in 100 ml of absolute acetonitrile is decomposed with 1.8 g of 1,5-diazabicyclo[5.4.0]undec-5-ene; it is then stirred for 1 hour at 20° to 25° C., diluted with 500 ml of water and acidified with hydrochloric acid. The precipitated oil is taken up with 200 ml of ethyl acetate, dried over sodium sulfate and concentrated by evaporation. Crystallisation of the oily residue from diethyl ether and acetone yields, as colourless crystals, N-[2-(2-ethoxy-ethoxy)-phenyl-sulfonyl]-N'-(4-difluoromethoxy-6-methyl-pyrimidin-2-yl)-urea, m.p. 90° to 95° C. (decomposition); yield 2.7 g.
後処理
- dry with materialdried over sodium sulfate
- concentrationconcentrated by evaporation
- customCrystallisation of the oily residue from diethyl ether and acetone
出典と根拠
- ORDレコード
- ord-8091d18f191449af81835a836d00e8b3
- 出典データセット
- uspto-grants-1984_10
- 特許番号
- US04480101
反応ノート
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