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Calcium Carbonate → HCID 20446511、化合物

HRID 2417753
ノート
印刷プレビュー

反応式

HRID 2417753 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 20446511HCID 20446511、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8d058a39995d47acae00c1beac708691
出典データセット
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04470826

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート