Cesium fluoride → HCID 22498336、化合物

HRID 1815523ノート

反応式

HRID 1815523 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 hours, 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 367 (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-b11962a8171447daa5028b00b2c2488f
出典データセット
uspto-grants-2005_04
特許番号
US06878700B1

反応ノート

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