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Water → t-Butyl 2-(6-cyano-2-naphthyloxy)-5-nitrobenzoate

HRID 895712
ノート
印刷プレビュー

反応式

HRID 895712 の反応式
F[C:2]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:3]=1[C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5].[C:18]([C:20]1[CH:21]=[C:22]2[C:27](=[CH:28][CH:29]=1)[CH:26]=[C:25]([OH:30])[CH:24]=[CH:23]2)#[N:19].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[C:18]([C:20]1[CH:21]=[C:22]2[C:27](=[CH:28][CH:29]=1)[CH:26]=[C:25]([O:30][C:2]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:3]=1[C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5])[CH:24]=[CH:23]2)#[N:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 45894766-Hydroxy-2-naphthonitrileHCID 22380964Tert-butyl 2-fluoro-5-nitrobenzoate

生成物 1

HCID 22380917t-Butyl 2-(6-cyano-2-naphthyloxy)-5-nitrobenzoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The compound (t-butyl 2-fluoro-5-nitrobenzoate) (1.74 g) obtained in a previous production example, 6-cyano-2-naphthol (1.86 g) and potassium carbonate (8.2 g) were heated to 50° C. in N,N-dimethylformamide and reacted for 2 hours. After cooling to room temperature, water was added and extraction was performed with ethyl acetate. The ethyl acetate layer was washed with saturated saline and dried over magnesium sulfate, and the solvent was distilled off. The residue was purified by silica gel chromatography (300 g, hexane:ethyl acetate=5:1) to obtain 3.23 g of t-butyl 2-(6-cyano-2-naphthyloxy)-5-nitrobenzoate.

後処理

  1. customreacted for 2 hours
  2. extractionextraction
  3. washThe ethyl acetate layer was washed with saturated saline
  4. dry with materialdried over magnesium sulfate
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel chromatography (300 g, hexane:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-963d3e736c7340afb56855abd981d7af
出典データセット
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06916837B2

反応ノート

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