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Pyridine → HCID 67493799, 화합물

HRID 1920725
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HRID 1920725 반응식
[NH2:1][C:2]1[O:6][N:5]=[C:4]([CH:7]([CH2:9][CH3:10])[CH3:8])[CH:3]=1.N1C=CC=CC=1.Cl[C:18]([O:20][CH2:21][C:22]([Cl:25])([Cl:24])[Cl:23])=[O:19]>C(Cl)Cl>[Cl:23][C:22]([Cl:25])([Cl:24])[CH2:21][O:20][C:18](=[O:19])[NH:1][C:2]1[O:6][N:5]=[C:4]([CH:7]([CH2:9][CH3:10])[CH3:8])[CH:3]=1
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 870632,2,2-Trichloroethyl chloroformateHCID 131682125-Isoxazolamine,3-(1-methylpropyl)-(9CI)

생성물 1

HCID 67493799HCID 67493799, 화합물수율 140.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 5-amino-3-sec-butylisoxazole (500 mg; 3.57 mmol; 1 equiv.) and pyridine (0.58 mL; 7.13 mmol; 2 equiv.) in DCM (30 mL) was added 0.74 mL (5.35 mmol; 1.5 equiv.) of 2,2,2-trichloroethyl chloroformate dropwise. The reaction mixture was stirred overnight at room temperature, then diluted with DCM, and washed sequentially with water, 1N HCL aqueous solution, saturated aqueous NaHCO3 solution and brine. The organic layer was dried over Na2SO4, filtered, and the filtrate was concentrated under reduced pressure. The residue, 1.58 g of (3-sec-Butyl-isoxazol-5-yl)-carbamic acid 2,2,2-trichloro-ethyl ester was isolated as a pale yellow oil, and used as is in the next step.

후처리

  1. washwashed sequentially with water, 1N HCL aqueous solution, saturated aqueous NaHCO3 solution and brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-31a1454daaa6444d8db40acfc82c5087
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08173638B2

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