Isobutylamine → HCID 21512169、化合物

HRID 1576347ノート

反応式

HRID 1576347 の反応式
[CH:1]([NH:4][C:5]1[C:18]2[C:17](=[O:19])[C:16]3[C:11](=[C:12]([OH:20])[CH:13]=[CH:14][CH:15]=3)[C:10](=[O:21])[C:9]=2[C:8](Br)=[CH:7][CH:6]=1)([CH3:3])[CH3:2].[CH2:23]([NH2:27])[CH:24]([CH3:26])[CH3:25]>CO.[Cu]Cl.S([O-])([O-])(=O)=O.[Cu+2]>[CH:1]([NH:4][C:5]1[C:18]2[C:17](=[O:19])[C:16]3[C:11](=[C:12]([OH:20])[CH:13]=[CH:14][CH:15]=3)[C:10](=[O:21])[C:9]=2[C:8]([NH:27][CH2:23][CH:24]([CH3:26])[CH3:25])=[CH:7][CH:6]=1)([CH3:3])[CH3:2]

参加物

6

反応物 2

HCID 6558IsobutylamineHCID 215121524-Bromo-5-hydroxy-1-[(1-methylethyl)amino]-9,10-anthracenedione

生成物 1

HCID 21512169HCID 21512169、化合物

試薬・触媒・溶媒 3

HCID 24462Copper Sulfate触媒HCID 62652Cuprous chloride触媒HCID 887Methanol溶媒

実験手順

10 Parts 1-isopropylamino-4-bromo-5-hydroxy-anthraquinone, 50 parts isobutylamine, 0.1 part each of copper(I) chloride and basic copper sulphate are boiled under reflux (appr. 70°) until only small amounts of starting material can be detected (appr. 2 hours are required). The mixture is diluted with 50 parts methanol, the precipitated needles are filtered off with suction in the cold, washed with methanol and hot water. It is also possible to filter off with suction without previous dilution with methanol. The 1-isopropylamino-5-hydroxy-4-isobutylamino-anthraquinone so obtained is sulphonated as follows:

後処理

  1. temperatureunder reflux (appr. 70°) until only small amounts of starting material
  2. custom(appr. 2 hours are required)
  3. filtrationthe precipitated needles are filtered off with suction in the cold
  4. washwashed with methanol and hot water
  5. filtrationto filter off with suction without previous dilution with methanol

出典と根拠

ORDレコード
ord-ca7141dec83d42a4928ee4c65c50480e
出典データセット
uspto-grants-1976_09
特許番号
US03980677

反応ノート

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