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Water → HCID 15729149、化合物

HRID 1656946
ノート
印刷プレビュー

反応式

HRID 1656946 の反応式
[C:1]([NH:4][C:5]1[S:6][C:7]([S:10][C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][CH:12]=2)=[CH:8][N:9]=1)(=[O:3])[CH3:2].[Cl-].[NH4+].O.O1CCCC1>C(O)C.[Fe]>[C:1]([NH:4][C:5]1[S:6][C:7]([S:10][C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)=[CH:8][N:9]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 251939N-(5-((4-(Hydroxy(oxido)amino)phenyl)thio)-1,3-thiazol-2-yl)acetamide

生成物 1

HCID 15729149HCID 15729149、化合物収率 79.5%

試薬・触媒・溶媒 2

HCID 23925Iron触媒
HCID 702
Ethanol
溶媒

実験手順

To a mixture of 2-acetylamino-5-(4-nitrophenylthio)thiazole (2.8 g) and ammonium chloride (0.3 g) in a mixture of ethanol (60 ml), water (30 ml) and tetrahydrofuran (20 ml) was portionwise added the iron powder (3 g) at 80° C. with stirring. The mixture was refluxed for 2.5 hours with stirring. The reaction mixture was filtered by suction and the filtrate was concentrated under reduced pressure. The residue was triturated with water, the precipitates were collected by filtration, washed with water and dried in vacuo to give 2-acetylamino-5-(4-aminophenylthio)thiazole (2.0 g, yield: 79.5%). mp: 255°-257° C. (dec.)

後処理

  1. temperatureThe mixture was refluxed for 2.5 hours
  2. stirringwith stirring
  3. filtrationThe reaction mixture was filtered by suction
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was triturated with water
  6. filtrationthe precipitates were collected by filtration
  7. washwashed with water
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-5c68793551164cc0a3944e500527a5cd
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05256675

反応ノート

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