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Water → 4,5-Diamino-2,6-dichloropyrimidine

HRID 1160094
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HRID 1160094 반응식
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([Cl:11])[N:5]=[C:4]([Cl:12])[N:3]=1.[H][H].O>CO.[Ni]>[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([Cl:11])[N:5]=[C:4]([Cl:12])[N:3]=1
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참가 물질

6

반응물 3

HCID 962WaterHCID 3508112,6-Dichloro-5-nitropyrimidin-4-amineHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 2400434,5-Diamino-2,6-dichloropyrimidine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

To a solution of 4-amino-2,6-dichloro-5-nitropyrimidine, prepared as described in a), in methanol (30 ml), was added Raney nickel freshly prepared from 500 mg of alloy. The reaction mixture was stirred 20 hours in the hydrogen atmosphere. Then a new catalyst, prepared from 500 mg of alloy, was added and the reaction mixture was stirred next 24 hours in the hydrogen atmosphere. The catalyst was removed, the reaction mixture was concentrated in vacuo and the residue was extracted with hot water. Product, which was obtained after cooling of the water solution, was purified by chromatography (SiO2, VI—1:1)

후처리

  1. customfreshly prepared from 500 mg of alloy
  2. customThen a new catalyst, prepared from 500 mg of alloy
  3. additionwas added
  4. customThe catalyst was removed
  5. concentrationthe reaction mixture was concentrated in vacuo
  6. extractionthe residue was extracted with hot water
  7. customProduct, which was obtained
  8. customwas purified by chromatography (SiO2, VI—1:1)

출처 및 근거

ORD 기록
ord-bbf78615fbb84d04a4247fe9d4e89db0
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07816350B2

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