4-Fluoro-3-nitrobenzotrifluoride → 1-(Tetrahydropyran-4-yl)amino-2-nitro-4-trifluoromethylbenzene

HRID 74150

反応式

HRID 74150 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[NH2:15][CH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1>N1C=CC=CC=1>[O:19]1[CH2:20][CH2:21][CH:16]([NH:15][C:2]2[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=2[N+:12]([O-:14])=[O:13])[CH2:17][CH2:18]1

参加物

4

反応物 2

HCID 677784-Fluoro-3-nitrobenzotrifluorideHCID 4192234-Aminotetrahydropyran

生成物 1

HCID 185098281-(Tetrahydropyran-4-yl)amino-2-nitro-4-trifluoromethylbenzene収率 90.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
98 °C

実験手順

A 3-neck flask (200 mL) was charged with 1-fluoro-2-nitro-4-trifluoromethylbenzene (1.59 g, 7.61 mmol), 4-aminotetrahydropyran (1.00 g, 9.89 mmol), and pyridine (16 mL), and this was stirred at 98° C. for 23 hours. The yellow oil produced was allowed to cool, distilled water (approx. 20 mL) was added with stirring, and the precipitated crystals were filtered off. These were washed with distilled water and dried with heating at reduced pressure to yield the title compound (2.00 g, 90.5% yield) as yellow crystals.

後処理

  1. customThe yellow oil produced
  2. temperatureto cool
  3. distillationdistilled water (approx. 20 mL)
  4. additionwas added
  5. stirringwith stirring
  6. filtrationthe precipitated crystals were filtered off
  7. washThese were washed with distilled water
  8. customdried
  9. temperaturewith heating at reduced pressure

出典と根拠

ORDレコード
ord-359360c049ef4f41afd2e711efcfdd3b
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

関連ノート

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