Trifluoroacetic anhydride → 4-chloro-2-fluoro-5-methyl-6-nitro-N-phenoxycarbonylaniline

HRID 1271753

反応式

HRID 1271753 の反応式
[Cl:1][C:2]1[C:17]([CH3:18])=[CH:16][C:5]([NH:6][C:7]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:8])=[C:4]([F:19])[CH:3]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.[N+:33]([O-])([O-:35])=[O:34].[NH4+].C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl.O>[Cl:1][C:2]1[C:17]([CH3:18])=[C:16]([N+:33]([O-:35])=[O:34])[C:5]([NH:6][C:7]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:8])=[C:4]([F:19])[CH:3]=1

参加物

7

反応物 4

HCID 9845Trifluoroacetic anhydrideHCID 22985Ammonium nitrate2 回HCID 516892Sodium BicarbonateHCID 186156474-chloro-2-fluoro-5-methyl-N-phenoxycarbonylaniline

生成物 1

HCID 186156464-chloro-2-fluoro-5-methyl-6-nitro-N-phenoxycarbonylaniline収率 103.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒2 回

実験手順

4-Chloro-2-fluoro-5-methyl-N-phenoxycarbonylaniline (7.1 g, 25.4 mmol) was dissolved in chloroform (68 ml) and trifluoroaceticanhydride (13.5 ml) and ammonium nitrate (2.4 g, 30.5 mmol) were slowly added with stirring at ambient temperature. The stirring was continued for 18 hr when a second batch of ammonium nitrate (0.4 g, 5 mmol) was added and stirring continued for 8 hr. Water was added and solution was neutralized by slow addition of sodium bicarbonate solution followed by extration with chloroform. Oganic layer was dried and evaporated under reduced pressure to afford an oily product (8.5 g) which was used for the next step without purification.

後処理

  1. stirringstirring
  2. waitcontinued for 8 hr
  3. customOganic layer was dried
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-7f98b4c60eb14eb697a7a31a58b278a0
出典データセット
uspto-grants-2007_04
特許番号
USRE039590E1

関連ノート

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