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Triethylamine → N-Carbamoyl-4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-methyl-N-methyl benzoic acid amide

HRID 878829
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HRID 878829 반응식
ClCC([NH:5][C:6]([N:8]([C:10](=[O:35])[C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH2:21][C:20]([C:26]3[CH:31]=[C:30]([Cl:32])[CH:29]=[C:28]([Cl:33])[CH:27]=3)([C:22]([F:25])([F:24])[F:23])[O:19][N:18]=2)=[CH:13][C:12]=1[CH3:34])[CH3:9])=[O:7])=O.C(N(CC)CC)C>CO>[C:6]([N:8]([CH3:9])[C:10](=[O:35])[C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH2:21][C:20]([C:26]3[CH:27]=[C:28]([Cl:33])[CH:29]=[C:30]([Cl:32])[CH:31]=3)([C:22]([F:25])([F:23])[F:24])[O:19][N:18]=2)=[CH:13][C:12]=1[CH3:34])(=[O:7])[NH2:5]
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참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 86654461N-chloroacetyl-N'-[4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-methylbenzoyl]-N'-methyl urea

생성물 1

HCID 66784361N-Carbamoyl-4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-methyl-N-methyl benzoic acid amide수율 90%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 0.40 g of N-chloroacetyl-N′-[4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-methylbenzoyl]-N′-methyl urea synthesized in Synthetic Example 27 and 0.04 g of triethylamine in 4 mL of methanol was stirred at room temperature for 2 hours. After the completion of the reaction, the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (gradient of 1:4 to 4:1) to obtain 0.31 g of the aimed product as white crystal.

후처리

  1. customAfter the completion of the reaction
  2. distillationthe solvent was distilled off under reduced pressure
  3. customThe residue was purified with silica gel column chromatography that

출처 및 근거

ORD 기록
ord-97c51a91148543bca3ac6452e7ec4c97
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987464B2

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