Cesium fluoride → HCID 22498336、化合物

HRID 984503ノート

反応式

HRID 984503 の反応式
[NH:1]1[CH2:13][CH2:12][CH2:11][CH:3]([C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5])[CH2:2]1.F[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N+:21]([O-:23])=[O:22].[F-].[Cs+]>C1(C)C=CC=CC=1.C(OCC)(=O)C>[N+:21]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[N:1]1[CH2:13][CH2:12][CH2:11][CH:3]([C:4]([O:6][C:7]([CH3:9])([CH3:10])[CH3:8])=[O:5])[CH2:2]1)([O-:23])=[O:22]

参加物

6

反応物 3

HCID 25953Cesium fluorideHCID 738951-Fluoro-2-nitrobenzeneHCID 42271713-Piperidinecarboxylic acid t-butyl ester HCl

生成物 1

HCID 22498336HCID 22498336、化合物収率 96.2%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of Example 437C (10.4 g, 56.1 mmol) in toluene (112 mL) was added 2-fluoronitrobenzene (6.0 mL, 56 mmol) and CsF (852 mg, 5.6. mmol). The reaction mixture was stirred under reflux conditions for 18 h, and allowed to cool to ambient temperature. The mixture was diluted with ethyl acetate (100 mL), washed with 10% HCl (2×50 mL), followed by brine (3×100 mL), then dried (Na2SO4) and evaporated in vacuo to obtain the title compound (16.5 g, 94%). MS (ESI) m/e 307 (M+H)+.

後処理

  1. washwashed with 10% HCl (2×50 mL)
  2. dry with materialdried (Na2SO4)
  3. customevaporated in vacuo

出典と根拠

ORDレコード
ord-19767238f58047c89c8fdb090d7edeb8
出典データセット
uspto-grants-2005_03
特許番号
US06867203B2

反応ノート

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