Water → 3-[4-chloro-2-(2-cyclopropanecarbonyldiazanyl)-6-fluoro-3-methoxyphenyl]-1-methyl-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione

HRID 1265394ノート

反応式

HRID 1265394 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[N:11]([CH3:20])[C:10]2=[O:21])=[C:4]([NH:22][NH2:23])[C:3]=1[O:24][CH3:25].[CH:26]1([C:29](Cl)=[O:30])[CH2:28][CH2:27]1.C(N(CC)CC)C.O>O1CCOCC1>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:17])([F:19])[F:18])[N:11]([CH3:20])[C:10]2=[O:21])=[C:4]([NH:22][NH:23][C:29]([CH:26]2[CH2:28][CH2:27]2)=[O:30])[C:3]=1[O:24][CH3:25]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 865859073-[4-chloro-2-diazanyl-6-fluoro-3-methoxyphenyl]-1-methyl-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione

生成物 1

HCID 865859083-[4-chloro-2-(2-cyclopropanecarbonyldiazanyl)-6-fluoro-3-methoxyphenyl]-1-methyl-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

3-[4-chloro-2-diazanyl-6-fluoro-3-methoxyphenyl]-1-methyl-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione (0.15 g, 0.4 mmol) was dissolved in dioxane (10 ml) and added with cyclopropanecarbonyl chloride (0.04 g, 0.4 mmol) and triethylamine (0.04 g, 0.4 mmol). After stirred for 1 hr, the mixture was poured into water (15 ml) and extracted with ethyl acetate (10 ml×3). Organic phase was washed with brine and dried over Na2SO4. Final purification involved column chromatography (silica gel, ether). Yield: 0.15 g, 0.34 mmol.

後処理

  1. extractionextracted with ethyl acetate (10 ml×3)
  2. washOrganic phase was washed with brine
  3. dry with materialdried over Na2SO4
  4. customFinal purification

出典と根拠

ORDレコード
ord-2785a4a1700e425485002815461e9ec8
出典データセット
uspto-grants-2003_04
特許番号
US06545161B2

反応ノート

読み込み中…