Methyl 3-amino-2-chloro-5-fluoro-4-methylbenzoate → 2,3-Dichloro-5-fluoro-4-methylbenzoic acid

HRID 34580

反応式

HRID 34580 の反応式
N[C:2]1[C:3]([Cl:14])=[C:4]([CH:9]=[C:10]([F:13])[C:11]=1[CH3:12])[C:5]([O:7]C)=[O:6].N([O-])=O.[Na+].[ClH:19]>Cl.Cl[Cu]>[Cl:14][C:3]1[C:2]([Cl:19])=[C:11]([CH3:12])[C:10]([F:13])=[CH:9][C:4]=1[C:5]([OH:7])=[O:6]

参加物

5

反応物 2

HCID 13657452Methyl 3-amino-2-chloro-5-fluoro-4-methylbenzoateHCID 86602196HCID 86602196、化合物

生成物 1

HCID 136574412,3-Dichloro-5-fluoro-4-methylbenzoic acid

試薬・触媒・溶媒 2

HCID 62652Cuprous chloride触媒HCID 313Hydrochloric Acid溶媒

実験手順

8 g of methyl 3-amino-2-chloro-5-fluoro-4-methylbenzoate are diazotized with NaNO2 /HCl in aqueous solution. This diazonium salt solution is added dropwise to a solution of 4.1 g of CuCl in 16 ml of concentrated HCl. The mixture is then warmed until no further gas is formed. After cooling, the solid which has precipitated is separated off and taken up in 30 ml of 50% strength EtOH. After addition of 2.3 g of NaOH, the mixture is boiled for 1 hour. After cooling to room temperature, the mixture is acidified with HCl and the solid which has precipitated is isolated. Melting point: 179°-80°. Yield: 5.2 g.

後処理

  1. temperatureThe mixture is then warmed until no further gas
  2. customis formed
  3. temperatureAfter cooling
  4. customthe solid which has precipitated
  5. customis separated off
  6. additionAfter addition of 2.3 g of NaOH
  7. customthe solid which has precipitated
  8. customis isolated

出典と根拠

ORDレコード
ord-b8e48d4c300a4eb88eedc02c00b64818
出典データセット
uspto-grants-1988_08
特許番号
US04762844

関連ノート

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