Isobutylamine → HCID 21512169, 화합물

HRID 1576347노트

반응식

HRID 1576347 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

HCID 21512169HCID 21512169, 화합물

시약·촉매·용매 3

HCID 24462Copper Sulfate촉매HCID 62652Cuprous chloride촉매HCID 887Methanol용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-ca7141dec83d42a4928ee4c65c50480e
출처 데이터셋
uspto-grants-1976_09
특허 번호
US03980677

반응 노트

불러오는 중…