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Benzene → HCID 86756104、化合物

HRID 1274820
ノート
印刷プレビュー

反応式

HRID 1274820 の反応式
C(O[CH:4](OCC)[C:5]#[C:6][CH3:7])C.Cl.C1C=CC=CC=1.[CH3:18][O:19][C:20]1[CH:25]=[C:24]([O:26][C:27]2[CH:32]=[CH:31][CH:30]=[C:29]([C:33]([F:36])([F:35])[F:34])[CH:28]=2)[N:23]=[C:22]([C:37]([NH:39][NH2:40])=[O:38])[CH:21]=1>C(OCC)(=O)C.O>[CH:4](=[N:40][NH:39][C:37](=[O:38])[C:22]1[CH:21]=[C:20]([O:19][CH3:18])[CH:25]=[C:24]([O:26][C:27]2[CH:32]=[CH:31][CH:30]=[C:29]([C:33]([F:34])([F:35])[F:36])[CH:28]=2)[N:23]=1)[C:5]#[C:6][CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 1377212-Butyn-1-al diethyl acetalHCID 70268884HCID 70268884、化合物

生成物 1

HCID 86756104HCID 86756104、化合物

試薬・触媒・溶媒 1

HCID 22728543Water ethylacetate溶媒

実験手順

2-butyne-1-al diethyl acetal (0.27 g, 0.000993×2 mol) was mixed with a 2N aqueous hydrochloric acid solution (about 3 ml) and 5 ml of benzene, and then the resultant mixture was stirred at about 70° C. for about 2 hours. After cooling to room temperature, the obtained mixture was mixed with 4-methoxy-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide (0.325 g, 0.000993 mol), and the resultant mixture was stirred at room temperature for 45 minutes. The obtained reaction solution was distributed in ethyl acetate-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. customThe obtained reaction solution
  2. customthe organic phase separated from the solution
  3. washwas washed with saturated brine
  4. dry with materialdried with anhydrous sodium sulfate
  5. concentrationconcentrated
  6. 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-08de3bf501d64b6e8d5c465ebbe5526a
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06159901

反応ノート

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