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

HRID 34580

반응식

HRID 34580 반응식
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]

참가 물질

5

반응물 2

HCID 13657452Methyl 3-amino-2-chloro-5-fluoro-4-methylbenzoateHCID 86602196Hydrochloride sodium nitrite

생성물 1

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

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b8e48d4c300a4eb88eedc02c00b64818
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762844

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