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p-Toluenesulfonic acid → HCID 59280191、化合物

HRID 1913196
ノート
印刷プレビュー

反応式

HRID 1913196 の反応式
CN(C)[CH:3]=[C:4]([C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)[C:5](OCC)=[O:6].[NH:17]([C:19]1[N:24]=[CH:23][C:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])=[CH:21][CH:20]=1)[NH2:18].C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)C>[O:6]=[C:5]1[N:17]([C:19]2[N:24]=[CH:23][C:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])=[CH:21][CH:20]=2)[NH:18][CH:3]=[C:4]1[C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1
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 6101p-Toluenesulfonic acidHCID 45089857Tert-butyl 6-hydrazinylpyridine-3-carboxylateHCID 687048643-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester

生成物 1

HCID 59280191HCID 59280191、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

2.2 g (10.0 mmol) of the compound from Example 2A are initially charged in 50 ml of ethanol. 2.1 g (10.0 mmol) of the compound from Example 15A and 380 mg (2.0 mmol) of p-toluenesulfonic acid are added, and the mixture is stirred under reflux for 16 h. The mixture is then cooled to 0° C., and the solid formed is filtered off and washed once with a little ethanol (batch 1). The mother liquor is concentrated and the residue is triturated with a little ethanol. The solid obtained is filtered off and washed once with ethanol (batch 2). The two solids batches are combined and dried under high vacuum. The solid is then stirred in tert-butyl methyl ether for 30 min, filtered off again and dried under high vacuum.

後処理

  1. temperatureunder reflux for 16 h
  2. customthe solid formed
  3. filtrationis filtered off
  4. washwashed once with a little ethanol (batch 1)
  5. concentrationThe mother liquor is concentrated
  6. customthe residue is triturated with a little ethanol
  7. customThe solid obtained
  8. filtrationis filtered off
  9. washwashed once with ethanol (batch 2)
  10. customdried under high vacuum
  11. stirringThe solid is then stirred in tert-butyl methyl ether for 30 min
  12. filtrationfiltered off again
  13. customdried under high vacuum

出典と根拠

ORDレコード
ord-9ec73413d77f491b989bf74bd407b94d
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609698B2

反応ノート

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