Hydrochloric Acid → 2-Amino-3-nitro-6-(2,2,2-trifluoro-ethoxy)-benzoic acid ethyl ester

HRID 18615

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HRID 18615 반응식
[H-].[Na+].[F:3][C:4]([F:8])([F:7])[CH2:5][OH:6].[CH2:9]([O:11][C:12](=[O:24])[C:13]1[C:18](F)=[CH:17][CH:16]=[C:15]([N+:20]([O-:22])=[O:21])[C:14]=1[NH2:23])[CH3:10].Cl>C1COCC1>[CH2:9]([O:11][C:12](=[O:24])[C:13]1[C:18]([O:6][CH2:5][C:4]([F:8])([F:7])[F:3])=[CH:17][CH:16]=[C:15]([N+:20]([O-:22])=[O:21])[C:14]=1[NH2:23])[CH3:10]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 2756434Benzoic acid, 2-amino-6-fluoro-3-nitro-, ethyl ester

생성물 1

HCID 686161072-Amino-3-nitro-6-(2,2,2-trifluoro-ethoxy)-benzoic acid ethyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

420 mg NaH (60% suspension in oil) were added to a solution of 2.16 mL (29.8 mmol) 2,2,2-trifluoro-ethanol in 5 mL THF. When the gas evolution ceased, 1.0 g (4.38 mmol) 2-Amino-6-fluoro-3-nitro-benzoic acid ethyl ester was added. The resulting mixture was stirred at 0° C. for 30 minutes and at room temperature for further 30 minutes. To this mixture were added 2 mL of a 6 M aqueous HCl-solution, and most of the solvent was removed under reduced pressure. The residue was mixed with 20 mL water and the resulting solid was collected and washed with water and then hexane. The obtained yellow crystalline material was dried under reduced pressure at 35° C. Yield: 1.22 g.

후처리

  1. custommost of the solvent was removed under reduced pressure
  2. additionThe residue was mixed with 20 mL water
  3. customthe resulting solid was collected
  4. washwashed with water
  5. customThe obtained yellow crystalline material was dried under reduced pressure at 35° C

출처 및 근거

ORD 기록
ord-72e6377cac6543abae76d361f020c377
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741341B2

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