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Tetrahydrofuran → 2-Butyroylamino-4-(4-nitrophenoxy)pyridine

HRID 387930
ノート
印刷プレビュー

反応式

HRID 387930 の反応式
[C:1](Cl)(=[O:5])[CH2:2][CH2:3][CH3:4].[NH2:7][C:8]1[CH:13]=[C:12]([O:14][C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=2)[CH:11]=[CH:10][N:9]=1.C(N(CC)CC)C.O1CCCC1>O>[C:1]([NH:7][C:8]1[CH:13]=[C:12]([O:14][C:15]2[CH:16]=[CH:17][C:18]([N+:21]([O-:23])=[O:22])=[CH:19][CH:20]=2)[CH:11]=[CH:10][N:9]=1)(=[O:5])[CH2:2][CH2:3][CH3:4]
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 8028TetrahydrofuranHCID 8471TriethylamineHCID 8855Butyryl chlorideHCID 229367164-(4-Nitrophenoxy)pyridin-2-amine

生成物 1

HCID 229366772-Butyroylamino-4-(4-nitrophenoxy)pyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Butyroyl chloride (0.93 ml) was added dropwise to a stirred solution of 2-amino-4-(4-nitrophenoxy)pyridine (1.0 g), triethylamine (1.8 ml) and tetrahydrofuran (20 ml) at room temperature. After stirring for 1 hour, water was added, extraction was performed with ethyl acetate, the extract was dried over magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (hexane:ethyl acetate=2:1) to obtain 0.6 g of the target substance as a colorless oil.

後処理

  1. extractionextraction
  2. dry with materialthe extract was dried over magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by silica gel chromatography (hexane:ethyl acetate=2:1)
  5. customto obtain 0.6 g of the target substance as a colorless oil

出典と根拠

ORDレコード
ord-9fa824a0ae0747188954ececcfc9e181
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08372981B2

反応ノート

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