Iodoethane → HCID 14692897, 화합물

HRID 1607598노트

반응식

HRID 1607598 반응식
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:9]=[C:10]([CH:14]=[C:15]([Cl:18])[C:16]=1[F:17])[C:11]([OH:13])=[O:12].[CH2:19](I)[CH3:20]>CN(C)C=O>[Cl:7][C:8]1[CH:9]=[C:10]([CH:14]=[C:15]([Cl:18])[C:16]=1[F:17])[C:11]([O:13][CH2:19][CH3:20])=[O:12]

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 199713033,5-Dichloro-4-fluorobenzoic acid

생성물 1

HCID 14692897HCID 14692897, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

Potassium carbonate (36 g, 0.26 mol) was added to a stirred mixture of 3,5-dichloro-4-fluorobenzoic acid (27.6 g, 0.13 mol), ethyl iodide (41.2 g- 0.26 moles) and dry dimethylformamide (300 ml) under nitrogen. The reaction was heated to 80° C. for 6 hours. The dimethylformamide was removed in vacuo and the residue treated with water (200 ml) acidified with dilute hydrochloric acid and extracted with ethylacetate (2×250 ml). The organic layer was washed with water, dried over magnesium sulphate and evaporated in vacuo, to give an orange oil which was purified by chromatography on silica, using a 4:1 mixture of petrol and diethylether as eluent. The pink oil obtained crystallised on standing, and washing with ice-cold 40-60 petrol gave white crystals of ethyl 3,5-dichloro-4-fluorobenzoate (29 g).

후처리

  1. customThe dimethylformamide was removed in vacuo
  2. additionthe residue treated with water (200 ml)
  3. extractionextracted with ethylacetate (2×250 ml)
  4. washThe organic layer was washed with water
  5. dry with materialdried over magnesium sulphate
  6. customevaporated in vacuo
  7. customto give an orange oil which
  8. customwas purified by chromatography on silica
  9. additiona 4:1 mixture of petrol and diethylether as eluent
  10. customThe pink oil obtained
  11. customcrystallised
  12. washwashing with ice-cold 40-60 petrol

출처 및 근거

ORD 기록
ord-0c83716a4d8f4c2ba1de31c9a4cc0133
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866078

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