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Triethylamine → 5-{2,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethyloxy]-benzoyloxy}-1,3-dimethylpyrazole

HRID 659931
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HRID 659931 반응식
[Cl:1][C:2]1[C:10]([O:11][CH2:12][CH2:13][N:14]2[CH:18]=[N:17][N:16]=[N:15]2)=[C:9]([Cl:19])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH3:20][N:21]1[C:25]([OH:26])=[CH:24][C:23]([CH3:27])=[N:22]1.C(N(CC)CC)C>O1CCCC1>[Cl:1][C:2]1[C:10]([O:11][CH2:12][CH2:13][N:14]2[CH:18]=[N:17][N:16]=[N:15]2)=[C:9]([Cl:19])[CH:8]=[CH:7][C:3]=1[C:4]([O:26][C:25]1[N:21]([CH3:20])[N:22]=[C:23]([CH3:27])[CH:24]=1)=[O:5]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 574372552,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoyl chlorideHCID 178429390HCID 178429390, 화합물

생성물 1

HCID 592816475-{2,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethyloxy]-benzoyloxy}-1,3-dimethylpyrazole수율 87.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

2,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoyl chloride (0.60 g) was dissolved in tetrahydrofuran (5 ml), this solution was added dropwise to a tetrahydrofuran (5 ml) solution of 1,3-dimethyl-5-hydroxypyrazole (0.22 g) and triethylamine (0.23 g) at 5° C. and the mixture was stirred at room temperature for 6 hours. After the reaction, the mixture was extracted with ethyl acetate (100 ml) and then washed with diluted hydrochloric acid and an aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off to obtain the desired 5-{2,4-dichloro-3-[2-(1H-tetrazol-1-yl)ethyloxy]-benzoyloxy}-1,3-dimethylpyrazole (0.65 g).

후처리

  1. customAfter the reaction
  2. extractionthe mixture was extracted with ethyl acetate (100 ml)
  3. washwashed with diluted hydrochloric acid
  4. dry with materialan aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulfate
  5. distillationEthyl acetate was distilled off

출처 및 근거

ORD 기록
ord-1fd6f5b04d554a348e268f894dbb74ba
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084398B2

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