Ammonium Chloride → 3-(4-Aminophenyl)isothiazolo[5,4-d]pyrimidin-4-amine

HRID 227619ノート

反応式

HRID 227619 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[N:16][C:17]=3[NH2:19])[S:12][N:11]=2)=[CH:6][CH:5]=1)([O-])=O.[NH4+].[Cl-]>[Fe].C(O)C.O>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[N:16][C:17]=3[NH2:19])[S:12][N:11]=2)=[CH:6][CH:5]=1

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 444147423-(4-Nitrophenyl)isothiazolo[5,4-d]pyrimidin-4-amine

生成物 1

HCID 444147433-(4-Aminophenyl)isothiazolo[5,4-d]pyrimidin-4-amine収率 97%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 19096565Water ethanol溶媒

実験手順

A mixture of Example 96F (0.95 g, 3.5 mmol), iron (0.78 g, 13.9 mmol), and NH4Cl (0.19 g, 3.5 mmol) in 9:1 ethanol/water (80 mL) was heated to 60° C. for 4 hours, cooled to room temperature, and filtered through a pad of diatomaceous earth (Celite®). The pad was washed with THF and the filtrate was concentrated. The concentrate was suspended in water and filtered. The filter cake was washed with water and dried to provide 0.82 g (97% yield) of the desired product.

後処理

  1. filtrationfiltered through a pad of diatomaceous earth (Celite®)
  2. washThe pad was washed with THF
  3. concentrationthe filtrate was concentrated
  4. filtrationfiltered
  5. washThe filter cake was washed with water
  6. customdried

出典と根拠

ORDレコード
ord-a460971fa4ed47fbad10cd78486f36e4
出典データセット
uspto-grants-2009_07
特許番号
US07560552B2

反応ノート

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