反応式
[CH:1]([NH2:4])([CH3:3])[CH3:2].N12CCCN=C1CCCCC2.CN(C)[C:18]1[O:19][C:20](=[O:28])[CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[N:23]=1>C1(C)C(C)=CC=CC=1>[CH:1]([N:4]1[C:20](=[O:28])[CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[NH:23][C:18]1=[O:19])([CH3:3])[CH3:2]参加物
5
実験手順
Isopropylamine (1.2 g, 20.3 mmol) and 1,8-diazabicyclo[5,4,0]undec-7-ene (DBU, 6 mL) are added to a solution of 2-dimethylamino-4-trifluoromethyl-6H-1,3-oxazin-6-one (4.0 g, 19.2 mmol) in xylene (34 mL). The resultant reaction mixture is held at 100° C. for 3 hours, cooled, washed with 5 wt. % HCl (40 mL), and extracted with ethyl acetate. The combined organic extracts are concentrated and triturated with heptane. The solids are filtered and dried to give the title product as a yellow powder (2.3 g, 54% yield, mp 127°-129° C.) which is identified by 1H NMR (DMSO-d6) δ6.11 (1H, s), 4.96 (1H, sp), 1.35 (6H, d); and 19F NMR δ−68.9 (s).
後処理
- customThe resultant reaction mixture
- temperaturecooled
- washwashed with 5 wt. % HCl (40 mL)
- extractionextracted with ethyl acetate
- concentrationThe combined organic extracts are concentrated
- customtriturated with heptane
- filtrationThe solids are filtered
- customdried
出典と根拠
- ORDレコード
- ord-d1f2986d2ff44b47bd6a20692eb54ba4
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06355796B1
関連ノート
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