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Calcium Carbonate → HCID 20446511, 화합물

HRID 2417753
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HRID 2417753 반응식
[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH2:4].C(=O)([O-])[O-].[Ca+2].Br.[Br:19][CH2:20][CH2:21][NH:22]C1C=CC=CC=1>O>[OH2:11].[BrH:19].[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH:4][CH2:20][CH2:21][NH2:22]
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참가 물질

5

반응물 3

HCID 10112Calcium CarbonateHCID 54879442-Methyl-5-nitrobenzene-1,4-diamineHCID 12606985N-(2-Bromoethyl)aniline--hydrogen bromide (1/1)

생성물 1

HCID 20446511HCID 20446511, 화합물

시약·촉매·용매 1

HCID 962Water용매3회

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온도
0 °C

실험 절차

A suspension of 0.05 mol (8.35 g) of 2-methyl-4-amino-5-nitroaniline and 0.035 mol (3.5 g) of calcium carbonate in 100 ml of water is heated beforehand on a boiling water-bath, whilst stirring. A solution of 0.07 mol (14.35 g) of β-bromoethylaniline hydrobromide in 20 ml of water is added gradually, whilst stirring. After heating for two hours on the boiling water-bath, the hot reaction medium is filtered. After cooling the filtrate for 24 hours at 0° C., the expected product, which has crystallised in the form of the hydrobromide, is filtered off. The crude product is washed with acetone and then recrystallised from boiling water. After filtration, washing with acetone and drying in vacuo, 2-methyl-4-amino-5-nitro-N-(β-aminoethyl)-aniline hydrobromide monohydrate is obtained.

후처리

  1. temperatureis heated beforehand on a boiling water-bath
  2. stirringwhilst stirring
  3. filtrationthe hot reaction medium is filtered
  4. customthe expected product, which has crystallised in the form of the hydrobromide
  5. filtrationis filtered off
  6. washThe crude product is washed with acetone
  7. customrecrystallised
  8. filtrationAfter filtration
  9. washwashing with acetone
  10. customdrying in vacuo

출처 및 근거

ORD 기록
ord-8d058a39995d47acae00c1beac708691
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04470826

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