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

HRID 840095
ノート
印刷プレビュー

反応式

HRID 840095 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-85ceb8881f0148d7b79e1914119d07d7
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06365584B1

反応ノート

読み込み中…

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