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Sodium Hydroxide → HCID 131728621、化合物

HRID 254260
ノート
印刷プレビュー

反応式

HRID 254260 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:10]2[O:14][CH:13]=[N:12][CH:11]=2)[CH:7]=[CH:8][CH:9]=1)([O-])=O.[OH-].[Na+]>[Zn].C(O)(C(F)(F)F)=O>[O:14]1[C:10]([C:6]2[CH:5]=[C:4]([NH2:1])[CH:9]=[CH:8][CH:7]=2)=[CH:11][N:12]=[CH:13]1.[NH2:1][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1
参加物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 14798Sodium HydroxideHCID 27370675-(3-Nitrophenyl)oxazole

生成物 1

HCID 131728621HCID 131728621、化合物収率 105.1%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 6422Trifluoroacetic acid溶媒

実験手順

1 g (5.26 mmol, 1 eq.) of 5-(3-nitrophenyl)oxazole and 10 mL of TFA are introduced into a 1 L flask. 1 g of zinc is carefully added in a plurality of batches. The mixture is stirred for 2 hours at room temperature then is poured over ice. Sodium hydroxide is slowly added until the medium becomes basic, and the medium is extracted with diethyl ether. The organic phase is washed with a 1 M solution of HCl and the impurities are extracted with diethyl ether. The aqueous phase is again basified with sodium hydroxide and the product is extracted with diethyl ether. The organic phases are combined, dried over MgSO4 and filtered. After concentration to dryness, 700 mg (yield=83%) of aniline 3-oxazol-5-yl-phenylamine are obtained, in the form of a beige solid. The product is used without subsequent purification.

後処理

  1. additionthen is poured over ice
  2. extractionthe medium is extracted with diethyl ether
  3. washThe organic phase is washed with a 1 M solution of HCl
  4. extractionthe impurities are extracted with diethyl ether
  5. extractionthe product is extracted with diethyl ether
  6. dry with materialdried over MgSO4
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-d8a88f9123b34ed9afbeef6fc4fe6f17
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07875609B2

反応ノート

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