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Acetic Anhydride → HCID 22049779、化合物

HRID 1830884
ノート
印刷プレビュー

反応式

HRID 1830884 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]1[N:9]=[C:10]([C:13]2[CH:18]=[C:17]([N+:19]([O-])=O)[CH:16]=[CH:15][C:14]=2[CH3:22])[S:11][CH:12]=1.[C:23](OC(=O)C)(=[O:25])[CH3:24]>C(O)(=O)C.C(OCC)(=O)C>[CH3:22][C:14]1[CH:15]=[CH:16][C:17]([NH:19][C:23](=[O:25])[CH3:24])=[CH:18][C:13]=1[C:10]1[S:11][CH:12]=[C:8]([C:3]2[CH:4]=[N:5][CH:6]=[CH:7][C:2]=2[CH3:1])[N:9]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 22049688HCID 22049688、化合物

生成物 1

HCID 22049779HCID 22049779、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

4-Methyl-3-[2-(2-methyl-5-nitrophenyl)-1,3-thiazol-4-yl]pyridine (100 mg) and reduced iron (180 mg) were suspended in acetic acid (2 ml)-acetic anhydride (0.04 ml) and the mixture was stirred at 70° C. for 4 hrs. The reaction mixture was diluted with ethyl acetate and the insoluble material was filtered off. The organic layer was neutralized with saturated aqueous sodium hydrogen carbonate. The organic layer was separated and concentrated by drying. The residue was subjected to silica gel column chromatography (eluent, hexane:ethyl acetate=1:1–0:1) for purification. Recrystallization from ethyl acetate gave the title compound (43 mg) as colorless powder crystals.

後処理

  1. filtrationthe insoluble material was filtered off
  2. customThe organic layer was separated
  3. concentrationconcentrated
  4. customby drying
  5. customThe residue was subjected to silica gel column chromatography (eluent, hexane:ethyl acetate=1:1–0:1) for purification
  6. customRecrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-f7a8c1bb048f4e6fb90d1a69a8893504
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07067537B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート