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

HRID 227619노트

반응식

HRID 227619 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 23925Iron촉매HCID 19096565Water ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a460971fa4ed47fbad10cd78486f36e4
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560552B2

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