Hydrochloric Acid → HCID 21287066, 화합물

HRID 358193

반응식

HRID 358193 반응식
[H-].[Na+].O[C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[C:6]([CH3:13])[CH:5]=1.[Cl:14][C:15]1[CH:16]=[C:17]([C:22]([F:25])([F:24])[F:23])[CH:18]=[CH:19][C:20]=1F.Cl.CN(C)C=[O:30]>O>[CH3:13][C:6]1[CH:5]=[CH:4][C:12]([O:30][C:20]2[CH:19]=[CH:18][C:17]([C:22]([F:25])([F:24])[F:23])=[CH:16][C:15]=2[Cl:14])=[CH:11][C:7]=1[C:8]([OH:10])=[O:9]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 684754-Hydroxy-o-toluic acidHCID 157153Benzene, 2-chloro-1-fluoro-4-(trifluoromethyl)-

생성물 1

HCID 21287066HCID 21287066, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of sodium hydride (2.3 g, 50% dispersion in mineral oil, prewashed with petroleum, b.p. 40°-60°) and 4-hydroxy-2-methylbenzoic acid (3.4 g) in dry N,N-dimethylformamide (30 ml) was stirred for thirty minutes, then treated with 3-chloro-4-fluorobenzotrifluoride (4.5 g). The mixture was heated at 130° for five hours, cooled, diluted with water, acidified with 2N hydrochloric acid and extracted with ethyl acetate. The extracts were washed with water and brine, dried and evaporated. The residue was recrystallised from petroleum (b.p. 80°-100°) to give 2-methyl-5(2-chloro-4-trifluoromethylphenoxy)-benzoic acid (2.06 g, m.p. 113°). A suspension of this material (1.34 g) in thionyl chloride (5 ml) was heated under reflux for one hour and the excess reagent removed in vacuo. The residue was dissolved in acetonitrile and again evaporated to give crude acid chloride.

후처리

  1. temperatureThe mixture was heated at 130° for five hours
  2. temperaturecooled
  3. extractionextracted with ethyl acetate
  4. washThe extracts were washed with water and brine
  5. customdried
  6. customevaporated
  7. customThe residue was recrystallised from petroleum (b.p. 80°-100°)

출처 및 근거

ORD 기록
ord-3fd1f6e933434511a7e2005f8f96d4d9
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04465508

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