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

HRID 1274816ノート

反応式

HRID 1274816 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-d3f072e4dd1d40f7b6aa90062e8d9b35
出典データセット
uspto-grants-2000_12
特許番号
US06159901

反応ノート

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