Water → 2-(4-Chloro-2-(tetrahydropyran-4-yl)aminonitrobenzen-5-yl)benzoxazole

HRID 74294ノート

反応式

HRID 74294 の反応式
[Cl:1][C:2]1[C:7]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][C:5]([N+:17]([O-:19])=[O:18])=[C:4](F)[CH:3]=1.[NH2:21][CH:22]1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1.O>C(#N)C>[Cl:1][C:2]1[C:7]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][C:5]([N+:17]([O-:19])=[O:18])=[C:4]([NH:21][CH:22]2[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)[CH:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 4192234-AminotetrahydropyranHCID 674987962-(4-Chloro-2-fluoronitrobenzen-5-yl)benzoxazole

生成物 1

HCID 674991902-(4-Chloro-2-(tetrahydropyran-4-yl)aminonitrobenzen-5-yl)benzoxazole収率 21%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 2-(4-chloro-2-fluoronitrobenzen-5-yl)benzoxazole (see Working Example 112-1) (0.38 g, 1.3 mmol) in acetonitrile (8 mL) was added 4-aminotetrahydropyran (0.30 g, 2.9 mmol), and this was heated to reflux for 2 hours. After the reaction was complete, this was cooled to room temperature, water was added, and the precipitated crystals were filtered. The crystals obtained were purified by silica gel column chromatography to yield the title compound (0.10 g, 21% yield) as brown crystals.

後処理

  1. temperaturethis was heated
  2. temperatureto reflux for 2 hours
  3. filtrationthe precipitated crystals were filtered
  4. customThe crystals obtained
  5. customwere purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f2b515ed9ff24eb585bd659ce4125e1c
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

反応ノート

読み込み中…