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Water → N6-{2-[(7-Chloro[1,2,4]triazolo[1,5-c]pyrimidin-5-yl)amino]ethyl}-3-nitropyridine-2,6-diamine

HRID 2389768
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HRID 2389768 반응식
Cl[C:2]1[N:7]2C=[CH:9][N:10]=[C:6]2[CH:5]=[C:4]([Cl:11])[N:3]=1.FC(F)(F)C(O)=O.[NH2:19][CH2:20][CH2:21][NH:22][C:23]1[N:28]=[C:27]([NH2:29])[C:26]([N+:30]([O-:32])=[O:31])=[CH:25][CH:24]=1.CC[N:35](C(C)C)C(C)C.O>CC(O)C>[Cl:11][C:4]1[N:3]=[C:2]([NH:19][CH2:20][CH2:21][NH:22][C:23]2[N:28]=[C:27]([NH2:29])[C:26]([N+:30]([O-:32])=[O:31])=[CH:25][CH:24]=2)[N:7]2[N:35]=[CH:9][N:10]=[C:6]2[CH:5]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 469421175,7-Dichloroimidazo[1,2-c]pyrimidineHCID 86641361N6-(2-aminoethyl)-3-nitropyridine-2,6-diamine trifluoroacetate

생성물 1

HCID 59312901N6-{2-[(7-Chloro[1,2,4]triazolo[1,5-c]pyrimidin-5-yl)amino]ethyl}-3-nitropyridine-2,6-diamine

시약·촉매·용매 1

HCID 3776
Isopropanol
용매

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온도
80 °C

실험 절차

194 mg (3.20 mmol) of 5,7-dichloroimidazo[1,2-c]pyrimidine are suspended in 8 ml of 2-propanol, and 403.9 mg (1.13 mmol) of N6-(2-aminoethyl)-3-nitropyridine-2,6-diamine trifluoroacetate and 331.7 mg (2.57 mmol) of DIPEA are added. The mixture is heated at 80° C. for 16 h. After this time, water is added, and the precipitate which separates out is filtered off with suction. It is washed with a little 2-propanol/water, and the resulting solid is dried under high vacuum. 265 mg (74% of theory) of the product are obtained as a solid.

후처리

  1. filtrationthe precipitate which separates out is filtered off with suction
  2. washIt is washed with a little 2-propanol/water
  3. customthe resulting solid is dried under high vacuum
  4. custom265 mg (74% of theory) of the product are obtained as a solid

출처 및 근거

ORD 기록
ord-4b2e0a96f8404917afdddc5541e54c57
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08273752B2

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