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4-Methylmorpholine → n-{3-Nitro-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide

HRID 840095
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HRID 840095 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:4][C:3]=1[N+:18]([O-:20])=[O:19].[F:21][C:22]([F:36])([F:35])[C:23]1[CH:24]=[C:25]([CH:28]=[C:29]([C:31]([F:34])([F:33])[F:32])[CH:30]=1)[CH2:26][NH2:27].CN1CCOCC1>CS(C)=O.C(OCC)(=O)C>[N+:18]([C:3]1[CH:4]=[C:5]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:11])=[O:10])[CH:6]=[CH:7][C:2]=1[NH:27][CH2:26][C:25]1[CH:28]=[C:29]([C:31]([F:32])([F:33])[F:34])[CH:30]=[C:23]([C:22]([F:21])([F:35])[F:36])[CH:24]=1)([O-:20])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 79724-MethylmorpholineHCID 5210993,5-Bis(trifluoromethyl)benzylamineHCID 4599069N-(4-fluoro-3-nitrophenyl)benzenesulfonamide

생성물 1

HCID 22621842n-{3-Nitro-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매
HCID 8857
Ethyl Acetate
용매

실험 절차

N-{4-fluoro-3-nitro-phenyl}-benzenesulphonamide (3.0 g, 10 mmol), 3,5-bis-trifluoromethylbenzylamine (3.0 g, 12.5 mmol) and N-methylmorpholine (2.2 mL, 20 mmol) in 25 mL dimethylsulphoxide are kept for 6 h at 60-100° C., diluted with 150 mL ethyl acetate, washed with water, dilute hydrochloric acid and water again, dried and concentrated by evaporation until not quite dry. The residue is combined with 80 mL EtOH and evaporated down to a residual volume of about 50 mL. The crystals precipitated after cooling are filtered off and washed with EtOH and petroleum ether.

후처리

  1. washwashed with water, dilute hydrochloric acid and water again
  2. customdried
  3. concentrationconcentrated by evaporation until not
  4. customquite dry
  5. customevaporated down to a residual volume of about 50 mL
  6. customThe crystals precipitated
  7. temperatureafter cooling
  8. filtrationare filtered off
  9. washwashed with EtOH and petroleum ether

출처 및 근거

ORD 기록
ord-85ceb8881f0148d7b79e1914119d07d7
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06365584B1

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