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Benzene → HCID 86756104, 화합물

HRID 1274820
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HRID 1274820 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 1377212-Butyn-1-al diethyl acetalHCID 70268884HCID 70268884, 화합물

생성물 1

HCID 86756104HCID 86756104, 화합물

시약·촉매·용매 1

HCID 22728543Water ethylacetate용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-08de3bf501d64b6e8d5c465ebbe5526a
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06159901

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