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Imidazole → 2-Amino-5-(4-[1-imidazolyl]-phenylsulfonyloxy)nitro-benzene

HRID 1823763
ノート
印刷プレビュー

反応式

HRID 1823763 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][S:9]([C:12]2[CH:17]=[CH:16][C:15](F)=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:4][C:3]=1[N+:19]([O-:21])=[O:20].[NH:22]1[CH:26]=[CH:25][N:24]=[CH:23]1>CN(C)C=O>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([N:22]3[CH:26]=[CH:25][N:24]=[CH:23]3)=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:4][C:3]=1[N+:19]([O-:21])=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 795ImidazoleHCID 120188434-Amino-3-nitrophenyl 4-fluorobenzenesulfonate

生成物 1

HCID 221470072-Amino-5-(4-[1-imidazolyl]-phenylsulfonyloxy)nitro-benzene収率 57.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

15.6 g of 2-amino-5-(4-fluorophenylsulfonyloxy)nitrobenzene were combined with 20.7 g imidazole in 100 ml dimethylformamide in a round bottom flask. The reaction mixture was heated to reflux for 3 hours and then cooled to room temperature. Reaction mixture was then precipitated by addition of water filtered and precipitate was washed with water and dried. Residue was resolubilized in hot ethyl glycol, crystallized by cooling and the crystals were washed with methanol and dried, yielding 10.4 g of 2-amino-5-(4-[1-imidazolyl]-phenylsulfonyloxy)nitro-benzene (melting point 209° C.).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 3 hours
  3. customReaction mixture
  4. customwas then precipitated by addition of water
  5. filtrationfiltered
  6. washprecipitate was washed with water
  7. customdried
  8. customcrystallized
  9. temperatureby cooling
  10. washthe crystals were washed with methanol
  11. customdried

出典と根拠

ORDレコード
ord-3ea7af849d4744a8acf784f28da004e9
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07041668B2

反応ノート

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