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Triethylamine → Methyl 2,4-dichloro-3-propoxyaminocarbonylbenzoate

HRID 377549
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HRID 377549 반응식
Cl[C:2]([C:4]1[C:5]([Cl:15])=[C:6]([CH:11]=[CH:12][C:13]=1[Cl:14])[C:7]([O:9][CH3:10])=[O:8])=[O:3].Cl.[CH2:17]([O:20][NH2:21])[CH2:18][CH3:19].C(N(CC)CC)C>C(Cl)Cl>[Cl:15][C:5]1[C:4]([C:2]([NH:21][O:20][CH2:17][CH2:18][CH3:19])=[O:3])=[C:13]([Cl:14])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12283955O-propylhydroxylamine hydrochlorideHCID 18517406Methyl 3-chlorocarbonyl-2,4-dichlorobenzoate

생성물 1

HCID 18517417Methyl 2,4-dichloro-3-propoxyaminocarbonylbenzoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

10.7 g (0.04 mol) of methyl 3-chlorocarbonyl-2,4-dichlorobenzoate in 100 ml of methylene chloride were slowly added dropwise at 30° C. to a solution of 4.50 g ((0.04 mol) of propoxyamine hydrochloride and 4.05 g (0.04 mol) of triethylamine in 200 ml of methylene chloride. After the reaction mixture had been stirred for 2 hours at room temperature, it was washed with dilute phosphoric acid, dried and concentrated. The residue obtained was chromatographed on silica gel (eluant:toluene/ethyl acetate=9/1). This gave 11.50 g of methyl 2,4-dichloro-3-propoxyaminocarbonylbenzoate.

후처리

  1. washit was washed with dilute phosphoric acid
  2. customdried
  3. concentrationconcentrated
  4. customThe residue obtained
  5. customwas chromatographed on silica gel (eluant:toluene/ethyl acetate=9/1)

출처 및 근거

ORD 기록
ord-abd1ecfc4d604b7e951b2e86972e0611
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06028035

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