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Triethylamine → 3-{3-[2-(2,4-Di-tert-amylphenoxy)butyramido]-benzamido}-5-butanoyloxy-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-1H-pyrazole

HRID 1660540
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HRID 1660540 반응식
[C:1]([C:6]1[CH:47]=[C:46]([C:48]([CH2:51][CH3:52])([CH3:50])[CH3:49])[CH:45]=[CH:44][C:7]=1[O:8][CH:9]([CH2:42][CH3:43])[C:10]([NH:12][C:13]1[CH:14]=[C:15]([CH:39]=[CH:40][CH:41]=1)[C:16]([NH:18][C:19]1[CH:23]([N:24]2[CH:28]=[CH:27][CH:26]=[N:25]2)[C:22](=[O:29])[N:21]([C:30]2[C:35]([Cl:36])=[CH:34][C:33]([Cl:37])=[CH:32][C:31]=2[Cl:38])[N:20]=1)=[O:17])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:60](OCl)(=[O:64])[CH2:61][CH2:62][CH3:63].C(OCC)(=O)C>O1CCCC1>[C:1]([C:6]1[CH:47]=[C:46]([C:48]([CH2:51][CH3:52])([CH3:49])[CH3:50])[CH:45]=[CH:44][C:7]=1[O:8][CH:9]([CH2:42][CH3:43])[C:10]([NH:12][C:13]1[CH:14]=[C:15]([CH:39]=[CH:40][CH:41]=1)[C:16]([NH:18][C:19]1[C:23]([N:24]2[CH:28]=[CH:27][CH:26]=[N:25]2)=[C:22]([O:29][C:60](=[O:64])[CH2:61][CH2:62][CH3:63])[N:21]([C:30]2[C:31]([Cl:38])=[CH:32][C:33]([Cl:37])=[CH:34][C:35]=2[Cl:36])[N:20]=1)=[O:17])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 136682733-{3-[2-(2,4-Di-tert-amylphenoxy)butyramido]benzamido}-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-5-oxo-2-pyrazolineHCID 18444075Butanoyloxy chloride

생성물 1

HCID 205569513-{3-[2-(2,4-Di-tert-amylphenoxy)butyramido]-benzamido}-5-butanoyloxy-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-1H-pyrazole

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

30.6 g of 3-{3-[2-(2,4-di-tert-amylphenoxy)butyramido]benzamido}-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-5-oxo-2-pyrazoline (prepared by the method described in German Patent Application (OLS) No. 2,536,191) was dissolved in 100 ml of tetrahydrofuran and 5 g of triethylamine was added. To the solution, a solution containing 3.5 g of butanoyloxy chloride dissolved in 10 ml of tetrahydrofuran was dropwise added. After the addition of the solution, the mixture was stirred for 1 hour. 500 ml of ethyl acetate was added to the reaction mixture and washed several times with water. The oil layer was dried with anhydrous sodium sulfate and concentrated. Upon crystallization of the residue from acetonitrile, 24 g of Coupler (5) was obtained. The melting point of the coupler was 63° to 68° C.

후처리

  1. additionwas dropwise added
  2. additionAfter the addition of the solution
  3. washwashed several times with water
  4. dry with materialThe oil layer was dried with anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customUpon crystallization of the residue from acetonitrile, 24 g of Coupler (5)
  7. customwas obtained
  8. customwas 63° to 68° C.

출처 및 근거

ORD 기록
ord-b3fad9f1cffc42d2ba9d9de60a7fb7f4
출처 데이터셋
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04308343

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