Benzene → 4-Ethylamino-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2,3,3,3-pentafluoropropylidene] hydrazide

HRID 1274816노트

반응식

HRID 1274816 반응식
[CH2:1]([NH:3][C:4]1[CH:9]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=2)[N:7]=[C:6]([C:21]([NH:23][NH2:24])=[O:22])[CH:5]=1)[CH3:2].O.[F:26][C:27]([F:34])([C:30]([F:33])([F:32])[F:31])[CH:28]=O.C1C=CC=CC=1.Cl>C(OCC)(=O)C.O>[F:26][C:27]([F:34])([C:30]([F:33])([F:32])[F:31])[CH:28]=[N:24][NH:23][C:21](=[O:22])[C:6]1[CH:5]=[C:4]([NH:3][CH2:1][CH3:2])[CH:9]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:18])([F:19])[F:20])[CH:12]=2)[N:7]=1

참가 물질

7

반응물 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 2776005HCID 2776005, 화합물HCID 702687404-Ethylamino-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide

생성물 1

HCID 867561004-Ethylamino-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2,3,3,3-pentafluoropropylidene] hydrazide

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

4-ethylamino-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide (0.30 g, 0.00088 mol) was mixed with 2,2,3,3,3-pentafluoropropionaldehyde monohydrate (0.29 g, 0.00088×2.0 mol) and benzene, and further with a small amount of concentrated hydrochloric acid. The obtained mixture was refluxed and dehydrated for about 8 hours using a water separator. The obtained reaction solution was distributed in ethyl acetate-saturated sodium bicarbonate water, and the organic phase separated from the solution was washed with saturated brine, dried with anhydrous sodium sulfate and then concentrated. The obtained concentrated solution was purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

후처리

  1. temperatureThe obtained mixture was refluxed
  2. customThe obtained reaction solution
  3. customthe organic phase separated from the solution
  4. washwas washed with saturated brine
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe obtained concentrated solution was purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-d3f072e4dd1d40f7b6aa90062e8d9b35
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06159901

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